Astm stp 640 1978

ADHESION MEASUREMENT OF THIN FILMS, THICK FI LMS, AN D BULK COATINGS A symposium presented at ASTM Headquarters AMERICAN SOCIETY FOR TESTING AND MATERIALS Philadelphia, Pa., 2-4 Nov 1976 ASTM SPECIAL TECHNICAL PUBLICATION 640 K L Mittal IBM Corporation East Fishkill Facility Hopewell Junction, N.Y editor List price $39.25 04-640000.25 AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race Street, Philadelphia, Pa 19103 Copyright BY AMERICANSOCIETYFOR TESTINGAND MATERIALS1978 Library of Congress Catalog Card Number: 77-84460 NOTE The Society is not responsible, as a body, for the statements and opinions advanced in this publication Foreword The symposium on Adhesion Measurement of Thin Films, Thick Films, and Bulk Coatings was held at the headquarters of the American Society for Testing and Materials, Philadelphia, Pa., 2-4 Nov 1976 The ASTM Publications Committee sponsored the symposium K L Mittal, IBM Corporation, presided as symposium chairman and editor of this publication Related ASTM Publications Spreading Resistance, STP 572 (1975), $3.55,04-572000-46 Surface Analysis Techniques for Metallurgical Applications, STP 596 (1976), $15.00, 04-596000-28 Composite Materials: Testing and Design (Fourth Conference), STP 617 (1974), $51.75, 04-617000-33 A Note of Appreciation to Reviewers This publication is made possible by the authors and, also, the unheralded efforts of the reviewers This body of technical experts whose dedication, sacrifice of time and effort, and collective wisdom in reviewing the papers must be acknowledged The quality level of ASTM publications is a direct function of their respected opinions On behalf of ASTM we acknowledge with appreciation their contribution A S T M Committee on Publications Editorial Staff Jane B Wheeler, Managing Editor Helen M Hoersch, Associate Editor Ellen J McGlinchey, Senior Assistant Editor Sheila G Pulver, Assistant Editor Contents Introduction GENERAL PAPERS RELATED TO ADHESION MEASUREMENT Adhesion Measurement: Recent Progress, Unsolved Problems, and Pmspeets K L MITTAL Discussion 16 Locus of Failure and Its Implications for Adhesion Measurements-S J GOOD Discussion 18 27 Problems in Adhesion Measurement j j BIKERMAN Discussion 30 38 Experimental Methods to Determine Locus of Failure and Bond Failure Mechanism in Adhesive Joints and Coattng-Substrate Combinations w L BAUN 41 Thin-Film Adhesion and Adhesive Failure -A Perspective D M MATTOX Discussion 54 62 Use of Fracture Mechanics Concepts in Testing of Film Adhesion-W D BASCOM, P F BECHER, J L BITNER, AND J S MURDAY Discussion 63 79 Techniques for Measuring Adhesive Energies in Metal/Ceramic Systems L E MURR Discussion 82 97 ADHESION MEASUREMENT OF T H I N FILMS Adhesion of Thin Plasma Polymer Films to Plastics-L W CRANE AND C L HAMERMESH Discussion Electromagnetic Tensile Adhesion Test Method soL KaONGELB Discussion 101 106 107 120 Measurements of Film-Substrate Bond Strength by Laser Spallation-J L VOSSEN 122 Discussion 131 Hardness and Adhesion of Filmed Structures as Determined by the Scratch Technique J AHN, K L MITTAL, AND R H MACQUEEN Discussion 134 156 Threshold Adhesion Failure: An Approach to Thin-Film Adhesion Measurement Using the Stylus M e t h o d - J OROSHNIKAND W K CROLL Discussion 158 182 Adhesion of Granular Thin FilmS -ROLAND FAURE Discussion 184 197 Adhesion Measurement on Thin Evaporated Filmsw KAIZO KUWAHARA,HIDENORI HmOTA, AND NOBUO UMEMOTO Discussion 198 207 ADHESION MEASUREMENT OF T r a c k FILMS Adhesion Measurements on Thick-Film Conduetors T T HITCH Discussion 211 231 Adhesion of Thick Films to Ceramic and Its Measurement by Both Destructive and Nondestructive M e a n s - - s L MOREY Discussion 233 250 Evaluation of Methods for Performing Adhesion Measurements of Thick.Film Terminations on Chip Components-G I E W E L L Discussion 251 267 Adhesion Measurement Technique for Soldered Thick-Film Conductors s s LEVEN Discussion 269 283 Adhesion of Flame-Sprayed Coatings -H s INGHAM, JR 285 Adherence Measurements and Evaluation of Thick-Film Platinum-Gold s SCHROTER 293 ADHESION MEASUREMENT OF DEPOSITS AND COATINGS Adhesion Testing of Deposit-Snbstrate Combinations-J w DINI AND H R JOHNSON Discussion Methods for Evaluating Adhesion of Photoresist Materials to Semiconductor Deviees r A DECKERT Discussion Effect of Aspect Ratio on Tensile Bond Strength for Butt Joint of Internal Fracture -Theoretical and Experimental Analysis-MINEO MASUOKA AND KAZUMUNE NAKAO Discussion Measuring the Temperature Dependence of the Strength of Metal-Polymer Jolnts N I EGORENKOV AND V A BELYI Peel Test for Determlning the Adhesion of Electrodeposits on Metallic Substrates o J KLINGENMAIER AND S M DOBRASH Discussion 305 326 327 341 342 359 362 369 389 SUMMARY Summary 393 Index 399 KLINGENMAIER AND DOBRASH ON THE PEEL TEST 387 pected that rupture would occur in the substrate during peeling and that the physical properties of the substrate would influence the peel strength This is true Plated plastics with good bond strength, when peeled, have been shown to rupture not at the interface but in a boundary layer within the plastic substrate [11] Since the physical strength of plastics is low, the peel strength must be necessarily low Plated metallic substrates with good bond strength when peeled, likewise, not rupture at the interface but in a boundary layer within the substrate For example, with nickel-plated aluminum alloy 3003, as much as 1.8 #m of the aluminum substrate was removed during peeling Since the physical strength of a metallic substrate is significantly greater than that of a plastic substratr the peel strength should also be relatively greater Peel strength ranges which were obtained with various nickel-plated substrates are presented in Fig as a function of the tensile strength of the substrate The extent of increased peel strength obtained by heating 150~ For h 600 [ - - I As Plated 350 Low Carbon Steel \ - 300 500 E (o z J=: 250 Coppe~(Hard) 400 - N 300 - _ 200 Aluminum \ ~ 150 ~ Grey Cast Iron -\ - 200 - I Wr~ 100 100 Lead-Tin 50 / l l l ) ] [ lO 140210 280 350420 4~ 560 Tensile Strength, MPa FIG Influence of tensile strength of substrate on peel strength of electrodeposited nickel after plating is shown by shaded areas With the exception of cast aluminum, where the rupture mechanism may differ from the wrought alloys, the maximum peel strengths obtained with the various plated substrates are shown to be directly proportional to the tensile strength of the substrate A ready prediction can then be made for the ultimate peel strengths possible with other substrates based on their tensile strength 388 ADHESION MEASUREMENT Summary and Conclusions A modified Jacquet peel test is a useful method to determine objectively and quantitatively the relative degree of adhesion of plated coatings on metallic substrates The test is helpful not only in evaluating various procedures for plating but in optimizing procedures or solutions to produce better adhesion Although a destructive test, it is recommended for monitoring production plating quality either by sacrificing parts or by running suitable test panels through the process Preparation of specimens for peel testing can be initiated after normal procedures for plating have been completed Most electroplated surfaces, if they can be overplated with an adherent coating of nickel, can be tested for peel strength Although the test is designed primarily for use with flat specimens, it can also be applied to cylindrical-shaped parts, such as pistons, when they are plated with a uniform thickness of the overlay and if they are rotated during peeling to maintain a 90 deg peel angle Primary test factors influencing peel results are the thickness of the overlay, the peel angle, and to a lesser extentmthe width of the peel strip The thickness of the overlay should be sufficient to resist tearing A thickness of 140 to 180 #m (0.0055 to 0.0071 in.) of sulfamate nickel is adequate for determining peel strengths up to 280 N/cm (160 lb/in.) When higher peel strengths are encountered, such as with plated steel substrates, proportionately thicker overlays are required to prevent tearing The force for peeling should be applied normal to the surface at a constant rate A peel width of 25 mm is recommended for optimum results References [1] Ferguson, A L and Stephan, E F., Monthly Review, American Electroplaters' Society, Vol 32, 1945, pp 894, 1006, 1116; Vol 33, 1946, pp 45, 166, 620 [2] Solov'eva, Z A and Vagramyan, A T., Electroplating and Metal Finishing, Vol 15, No 3, 1962, p 84; Vol 15, No 4, 1962, p 120 [3] Davies, D and Whittaker, J A., MetallurgicalReviews, Vol 12, 1967, pp 15-26 [4] Mittal, K L in Properties of Electrodeposits, Their Measurement and Significance, R Sard, H Leidheiser, Jr., and F Ogburn, Eds., The Electrochemical Society, Princeton, N.J., 1975, Chapter 17, pp 273-306 [5] Dini, J W and Johnson, H R., Proceedings, 18th Annual Conference, Society of Vacuum Coaters, 1975, pp 27-41 [6] Jacquet, P H., Transactions, The Electrochemical Society, Vol 66, 1934, p 393 [7] Brenner, A and Morgan, V D., Proceedings, 37th Annual American Electroplaters' Society, 1950, pp 51-65 [8] Linford, H B and Venkateswarlu, A., Plating, Vol 45, 1958, p 728 [9] Wittrock, H J and Swanson L., Plating, Vol 49, 1962, p 880 [10] Such, T E and Wyszynski, A E., Plating, Vol 52, 1965, p 1027 [11] Saubestre, E B., Durney, L D., Hajdu, J., and Bastenbeck, E., Plating, Vol 52, 1965, p 982 [12] McNamara, J B and Sexton, J., Paper No 995B presented to the Society of Automotive Engineers at the Detroit Meeting, Jan 11-15, 1965 KLINGENMAIER AND DOBRASH ON THE PEEL TEST 389 [13] Wittrock, H J., Proceedings 48th Annual American Electroplaters' Society, 1961, pp 52-59 [14] Mohler, J B and Shaefer, R M., Monthly Review, American Electroplaters' Society, Vol 34, 1947, pp 1361-1364 [15] Shreider, A V in Theory and Practiceof Chromium Electroplating, A T Vagramyan and N T Kudryavtscv, Eds., Israel Program for Scientific Translations, Ltd., Jerusalem, 1965, pp 55-60 DISCUSSION Carl Dahlquistl(written discussion ) Do the ribbons undergo ductile yield during the peeling? If so, it would be difficult to estimate the interfacial stress from application of peel mechanics O J Klingenmaier and S M Dobrash (authors' closure ) Measurements were not made in situ to determine elasticity of the strip during peeling, and permanent elongation was not normally encountered with the nickel strips However, in instances of extremely high peel strength, > 350 N / c m (200 lb/in.), stretch marks about mm long were produced on the strips during peeling H E Ashton2(written discussion) Have you investigated the angle of peeling, because most adhesive pull tests are carried out at 180 deg and the adhesion group of ASTM D-1 did not find any difference between 90 deg and 180 deg for the tape test, ASTM Measuring Adhesion by Tape Test (D 3359-74), with organic coatings O J Klingenmaier and S M Dobrash (authors" closure) Using a peel angle of 180 deg was not practical It was necessary to peel a strip over half its length at a lesser angle to position the jaws of the peeling device for a 180 deg pull Peel results showed much greater variation at 180 deg and were as much as 40 deg greater than that obtained at an angle of 90 deg Apparently, higher peel strengths obtained at an angle of 180 deg may be caused by the force required to bend the nickel overlay through an additional 90 deg In 13M Company, St Paul, Minn 55101 2National ResearchCouncilof Canada, Divisionof Building Research, Ottawa, Ont Canada 390 ADHESION MEASUREMENT the tape test for organic coatings, significantly less force is required to bend the overlay since it is thinner and more flexible than the nickel deposit used here J J Bikerman3(written discussion) The dependence of the peel strength on the width of the ribbon, which, by the way, I observed nearly 20 years ago, should be important for those who try to determine the peel strength by pulling at a bent wire The diameter of the wire certainly is in the range in which this strength is affected by the width; thus, comparison of results obtained with different wires may afford misleading information O J Klingemaier and S M Dobrash (authors' closure) Yes, we would expect the diameter of the wire to influence the results H E Hintermann4(written discussion) The various treatments and cleaning procedures applied to the substrate surface before coating influence the peel strength Among them, has glow discharge cleaning in inert or reactive gaseous atmospheres been considered (plasma etch)? If so, what were the results? O J Klingemaier and S M Dobrash (authors' closure) Glow discharge cleaning in inert atmosphere followed by vapor or ion deposition of a suitable metal has been considered for preparing difficult-to-plate metals for electrodeposition but has not yet been investigated 3Department of ChemicalEngineering,Case Western ReserveUniversity,Cleveland,Ohio 44106 4LaboratoireSuissede RecherchesHologeres,Ch - 2000 Neuchatel, Switzerland Summary STP640-EB/Jan 1978 Summary This volume containing 25 papers brings together the state of the art pertaining to adhesion measurement techniques for a variety of thin films, thick films, and coatings Mittal, in the introductory paper, has discussed at length some of the problems and controversies involved in adhesion measurement He has suggested the use of the term "practical adhesion" to denote forces or the work required to disrupt an adhering system (adherend-adherate combination) irrespective of the locus of failure, unless the failure is clearly in the bulk of one of the adhering phases Failure in bulk constitutes a case of cohesive failure, and is a measure of the cohesive strength of that particular phase References are made to the recent comprehensive reviews regarding adhesion measurement of thin films, thick films, and bulk coatings; and developments pursuant to these reviews are covered Some recommendations for future developments in the area of adhesion measurement are highlighted The importance of establishing the locus of failure in an adhering system is quite manifest in understanding the failure mechanism as well as to prescribe a proper remedy Good has described the level of possibility of true interfacial separation based on two theories [weak boundary layer (WBL) theory and theory based on fracture mechanics] and has critiqued both these theories Good points out that a case sometimes exists which mimics WBL failure in systems where no such material is present Failure propagates close to, but not at, the phase boundary because of mechanical reasons Bikerman has promulgated for a long time that true interfacial separation rarely, if ever, occurs What is taken as an apparent separation at the interface is a separation in the WBL In the present paper, he still adheres to his original ideas and cites some recent results to bolster his arguments In any case, the controversy apropos of the possibility of interfacial separation still persists, and it does not appear that it will be resolved, at least in the near future Also, Bikerman has criticized some of the so-called adhesion tests for latex paints on the grounds that these simply measure the cohesive strength of the paints The paper by Baun describes experimental methods to determine the locus of failure in an adhesive joint as well as in adhering systems The techniques discussed include ion scattering spectrometry (ISS), secondary 393 Copyright* 1978 by ASTM lntcrnational www.astm.org 394 ADHESION MEASUREMENT ion mass spectrometry (SIMS), scanning electron microscopy (SEM), Auger electron spectroscopy (AES), and electron spectroscopy for chemical analysis (ESCA); their advantages and limitations are discussed Mattox has reviewed the various factors which affect thin-film adhesion, and the importance of interfacial regions (in metallic adhering systems) in the measured adhesion of thin films is discussed He points up that an adhesion testing program must be designed to subject the film-substrate couple to the stresses which it will encounter in production and in service Bascom, Becher, Bitner, and Murday discuss the use of fracture mechanics concepts in the testing of film adhesion, and constant-compliance and applied-moment double-cantilever beam tests for adhesive fracture energy have been adapted for the measurement of adhesion of thick-film metallization on alumina substrates The thick-film tests involve beams soldered to metallization strips and measure the strain energy release rate, ~'c The fracture results are compared with peel strengths from solder-wire peel tests of the same metallizations The constant-compliance and the peel test data exhibit a bimodal distribution The advantages of the fracture mechanics approach are discussed Murr has determined the variation of adhesive energy of metal-ceramic [nickel on thorium dioxide (ThO2), nickel/chromium (80/20) on ThO2, and iron/nickel/chromium on aluminum oxide (A1203)] systems with temperature What Murr refers to as "adhesive energy" is more commonly known as thermodynamic work of adhesion, HI= Such determination of Wa should be helpful in predicting the practical adhesion between coatings of these metals on ceramic substrates The next seven papers deal with the adhesion of thin films Crane and Hamermesh have studied the adhesion of thin (1400 A) plasma polymerized films of styrene and acrylonitrile deposited on a number of plastics Adhesion of these films was measured by applying a 1/2 by in piece of Scotch No 810 tape to the fdm and then removing the tape in a 90-deg peel Krongelb describes a new technique for measuring practical adhesion of a thin-film structure without requiring any mechanical attachment to the film, and results are presented for evaporated copper film on thermally oxidized silicon The technique involves application of a known tensile stress to the film; the stress is developed by the interaction of an external magnetic field with an electric current through a suitably patterned specimen of the film to be evaluated The maximum stress which can be produced is limited by the available magnetic field, the fabrication of the test procedure, and the heating effect of the current through this structure It is shown that useful stresses of at least 24 000 psi are practical by the electromagnetic method Another technique, known as "laser spallation," which does not require any mechanical attachment is described by Vossen The technique involves SUMMARY 395 impinging a high-energy pulsed laser beam on the back side of the substrate; if the substrate is transparent, then a thick absorbing layer is first deposited on its back side By increasing the incident laser power, one can find a threshold at which the film is torn loose from the substrate The film is patterned into dots of about the same diameter as the incident laser beam If suitable corrections are applied, then it is claimed that the threshold energy can be related directly to the bond strength between the film and the substrate Spallation thresholds are given for various metal films on fused silica substrates The paper by Ahn, Mittal, and MacQueen discusses in the first part the evolution of the scratch technique for measuring practical adhesion of thin films and the difficulties involved in the interpretation of the results These authors describe the use of a very sensitive surface profilemeter, and a SEM coupled with energy dispersive X-ray spectroscopy to examine scratch topography, modes of film deformation, and the mechanism of film material removal during their studies of scratch hardness and adhesion of multilayer structures using a single point loaded scratch tester It is found that the scratch behavior is not as simple and general as was originally suggested by Weaver and co-workers The next paper, by Oroshnik and Croll, also deals with the scratch technique They have introduced the concept of Threshold Adhesion Failure (TAF) and the operational definition of TAF as adopted by the authors reads: Threshold Adhesion Failure occurs if, within the boundaries of a scratch and over its 1-cm path, removal of the film from its substrate can be detected by transmitted light with a microscope (magnification x 40) at even one spot, no matter how small The TAF criterion differs from the complete removal criterion as was orginally discussed by Weaver and coworkers The scratch test as used in the TAF mode has been shown to be very sensitive, capable of good reproductibility, and TAF loads are relative values that give some indication of the quality of film adherence Data are presented for aluminum films on fused quartz Faure describes a dynamic (ultrasonic vibration) method for measuring the adhesion of microscopic metallic grains which constitute granular thin films Data are presented for the adhesion of granular silver films deposited on carbon Also the adhesion of thick silver films on carbon is discussed Kuwahara, Hirota, and Umemoto present their results on the adhesion of thin aluminum and silver films on mild steel and glass, as measured by two techniques One is to pull down and the other is to twist off a rod whose bottom is cemented to the film with epoxy The critical force or the torque required to strip off the film from the substrate is taken as a measure of adhesion The next six papers deal with the adhesion of thick-film conductors In the first part of his paper, Hitch briefly reviews the adhesion measurement 396 ADHESION MEASUREMENT of thick-film materials and describes the particular requirements of thickfilm technology for test methods to measure the adhesion strength of these materials A number of test methods are treated with reference to their usefulness and practicability The second part of the paper is devoted to the review of two thick-film adhesion tests and data obtained using these at RCA laboratories These tests are the thermocompression bonded peel test and the soldered-wire peel test According to the author, the first test has been used successfully for adhesion strength measurement on gold- and silver-based conductor films Morey has evaluated two techniques for adhesion measurement of thick films on alumina One method is to solder an interconnection onto a thick film pad and measure the strength using a force gage Another method is to use a wire peel test The factors affecting adhesion values as obtained by these techniques are discussed Ewell has compared the nailhead lead tension and the ribbon lead shear tests for adhesion measurement of thick-film, solderable end terminations on chip resistors, and multilayer monolithic ceramic capacitors The criteria for test method evaluation are discussed The nailhead method is compatible with vendor data, and specimens can be easily and quickly prepared Leven describes the use of the pull test for measuring the adhesion of conductor-substrate combinations using soldered copper pins to conductor pads Also, the effects of four environmental stresses on the loss of adhesion are discussed, and it is concluded that the temperature cycling stress appears to be the most practical stress as a screening procedure for solder leaching, which leads to adhesion degradation Ingham discusses the considerations involved in testing the bond strength of flame-sprayed coatings and has presented the results (on two different flame sprayed coatings) of round-robin tests for the ASTM Method C 633-69 Schroter describes a pull-peel at 90-deg test for measuring adhesion of conductors and discusses the factors which affect conductor adhesion The next five papers deal with a variety of coatings Dini and Johnson have described the ring shear, conical-head tension, and I-beam tension tests for quantitative measurement of the adhesion of a number of electrodeposited coating-substrate combinations The pros and cons of each test are discussed, and adhesion data for various deposit-substrate combinations are included Deckert has used resistance to fluoride-containing etchant undercutting as a measure of relative adhesion of photoresist/SiO2 composites An empirical equation is given which approximately describes the shape of the undercut oxide edges, thus allowing a numerical measure of the relative adhesion A variation of this test can be used to detect nonuniform adhesion across a wafer surface SUMMARY 397 Masuoka and Nakao describe a general formula for tensile bond strength for the butt joint of internal fracture in terms of a simplified model constructed from measurable parameters The equations developed indicate that the bond strength depends on both the yield strength and the aspect ratio of the adhesive Egorenkov and Belyi discuss the temperature dependence of adhesion, as measured by the peel test, in metal-polymer joints employing temperature gradient in the plane of contact The strength of adhesion in the case of crystalline polymers is lower than that of amorphous ones, and decreases with increasing test temperature The final paper by Klingenmaier and Dobrash describes the use of the Jacquet peel test for determining the adhesion of plated coatings on metallic substrates The factors affecting peel values are discussed, and a relationship between the tensile strength of the substrate and the possible maximum peel strength is established Use of the peel test is demonstrated on a production part As a group, these papers provide a useful source of information and a guide for further development anent adhesion measurement techniques Although there are many unanswered questions and moot issues in the realm of adhesion measurement, the brisk activity and interest in this area is quite patent from this collection of papers The contents of this volume should be of interest to scientists, engineers, technologists, and production and manufacturing personnel whose work involves knowledge of adhesion of thin films, thick films, and coatings Also, this volume should be utile to both veteran (as a reference source) and novice (as a starting point) in this important area of adhesion measurement K L Mittal East FishkUl Facility, IBM Corporation, HopewetlJunction, N.Y 12533;symposium chairman and editor STP640-EB/Jan 1978 Index A Adherate, Adherend, Adhering system, Adhesiogram, 362 Adhesion Basic, 7, 9, 10 Fundamental, Good, 54 Interfacial, Practical, Tr~le, Adhesion, definition of, 6, Adhesion conversion factors, 17 Adhesion degradation due to environmental stress, 277-282 Adhesion, temperature dependence of, 362 Adhesion measurement techniques (for additional techniques, see References on pp 11-13) Applied moment double cantilever beam, 63 ASTM Method C 297-61, 287 ASTM Method C 633-69, 285 Conical head tension, 312-316 Constant compliance, 63 Electromagnetic tensile, 107-119 I-beam, 316-323 IBM dot, 220 Laser spallation, 122-131 Nailhead lead tension, 252 Parallel gap welding, 216 Peel, 217, 362-368, 369-389 Pull, 238, 375 Pull-down, 19%206 Pull-on-loop, 240 Pull-peel at 90-deg, 293 Push, 236 Ribbon lead shear, 252 Ring shear, 306-312 Scratch, 134-156 Scratch in threshold adhesion failure mode, 158-181 Shear bond, 287 Soldered-wire tension peel, 218, 227 Tensile bond, 287 TC peel, 221 Twisting-off, 199-206 Ultrasonic vibration, 184-196 Uniaxial tension, 215 Wire bond, 215 Wire peel, 239 Adhesion of Aluminum films on quartz, 166 Aluminum oxide coating, 290 Evaporated copper on SiO2, 107 Filmed structures, 149-156 Flame-sprayed coatings, 285-292 Gold and silver based conductor films, 211-230 Granular silver films on carbon, 184 Granular thin films, 184-195 Metal or alloys on metals or alloys, 305-324 Metal-ceramic systems, 82-97 399 Copyright*1978by ASTMInternational www.astm.org 400 ADHESION MEASUREMENT Metal film on mild steel, 198 Metals on Si02, 129 Metal-polymer joints, 362-368 Molybdenum coating, 291 Organic films, 150-151 Photoresist materials to semiconductors, 327-340 Plasma polymerized films, 103 Plated coatings on metallic substrates, 369-389 Polymers, 362-368 Soldered thick-film conductors, 269-282 Thick coatings, 13, 31-33, 285292, 305-325, 362-367, 369389 Thick films, 12-13, 63-79, 211230, 233-249, 251-266, 269282, 293-302 Thick film metalization on alumina, 63-78 Thick film Pt-Au, 293-302 Thick film terminations on chip components, 251-266 Thin films, 11-12, 54-60, 101105, 107-119, 122-131, 134156, 158-181, 184-197, 198206 Adhesive energies and temperature, 82-97 Adhesive energies in metal-ceramic systems, 82-97 Adhesive failure, 34-35 Adhesives, 347 Adhint, Angle of peeling, 378 Aspect ratio, 342 Auger electron spectroscopy, 47 B Basic adhesion, 7, 9, 10 Butt joints, 342 C ASTM Method C 297-61,285 ASTM Method C 633-69, 285 Characterization methods, 43-53 Chip components, 251-266 Cohesive failure, Comparison of surface characterization methods, 45 Conical head tension test, 312-316 Constant compliance fracture test, 65-67 Contact angle between metals and ceramics, 82-97 Contraction ratio, 355 Conversion factors, 17 Crescent fracture, 172, 176 Critical load, 135 D Dielectric, 328 E Electric current, 107 Electrodeposited metals, 305-324 Electromagnetic test, 10%119 Energy dispersive X-ray spectroscopy, 140, 233 Epoxy, 199 Etchants, 327 F Failure locus Possible regions for, 20 Practical importance of, 19-20 Filmed structures Adhesion of, 149-156 Hardness of, 141-149 Flame-sprayed coatings, 285-292 Fluoride etchants, 327 Force gage, 236 Fracture energy, 64 INDEX Fracture mechanics, 24-25 Fracture mechanics in film adhesion testing, 63-79 Friction, 179 Future developments in adhesion testing, 13 G Grain adhesion, 185 Granular thin films, 184-197 H Hexamethyldisilazane (HMDS), 327 I IBM dot test, 220 I-beam test, 316-323 Ideal practical adhesion test, 11,213 Interface, Interracial bonding, 57 Interfacial changes, time dependent, 59 Interfacial fracture, 58-59 Interfacial regions, 8, 55-57 Interfacial separation Theories regarding possibility of, 20-25 Inteffacial stress, 57-58 Internal fracture, 349 Interphases, Ion scattering spectroscopy, 44 J Jacquet peel test, 369 L Laser spallation method, 122-131 Locus of failure, 48 M Magnetic field, 107 Metal-polymer joints, 363-367 Microtopographer trace, 147 401 N Nailhead lead tension test, 252 P Parallel gap welding test, 216 Peel tests, 217 Photoresist adhesion, 327-340 Polymer films, 101-106 Poisson's ratio, 357 Practical adhesion Definition of, Factors affecting, 10 Relationship between basic adhesion and, 10 Proper joints, 36-37 Puil-down method, 199-206 Pull-on-loop method, 240 Pull-peel at 90-deg test, 293 Pull test, 238, 275 Push test, 236 R Ribbon lead shear test, 252 Ring shear test, 306-312 Round robin tests, 289 S Scanning electron microscopy, 44 Scratch hardness, 135, 141 Scratch technique, 134-156 Evolution of, 135-138 In threshold adhesion failure mode, 158-181 Secondary ion mass spectroscopy, 44 Sessile drop, 82 Shear bond test, 287 Silicon dioxide, 327 Solder-bond peel test, 69 Soldered thick-film conductors, 269 Soldered-wire tension-peel test, 218, 227 Spallation threshold, 129 Speed of peeling, 378 402 ADHESION MEASUREMENT Strain energy release rate, 63 Stress analysis, 343-346 Stress waves in solids, 124 Surface characterization methods, 43-53 T Tape test, 103 TC peel test, 221 Temperature coefficient, 82 Temperature dependence of adhesion, 362 Tensile bond strength, 342 Tensile bond test, 287 Termination adhesion, 256 Thick coatings, 13, 31-33,285-292, 305-325, 362-367, 369-389 Thick films, 12-13, 63-79, 211-230, 233-249, 251-266, 269-282, 293-302 Thin films, 11-12, 54-60, 101-105, 107-119, 122-131, 134-156, 158-181, 184-197, 198-206 Thin plasma polymer films, 101-106 Threshold adhesion failure, (TAF), 160 Threshold adhesion failure loads, 166 Twisting-off method, 199-206 Types of adhesion tests, 213 U Ultrasonic vibration test, 184-196 Undercutting, 329 Uniaxial tension tests, 215 Unitek micropull tester, 296 W Weak boundary layers (WBL), 9, 35-36 Weak boundary layer theory Critique of, 22-24 Wettability of polymeric substrates, 103 Wire bond test, 215 Wire peel test, 239 X X-ray photoelectron spectroscopy, 47 Y Yield strength, 348 Z Zero-creep, 82