Metallography And Microstructure Of Ancient And Historic .
METALLOGRAPHYANDMICROSTRUCTUREOFANCIENTANDHISTORIC METALS
METALLOGRAPHYANDMICROSTRUCTUREOFANCIENTANDHISTORIC METALSDAVID A. SCOTTTHEINTHEAGES EBSUTOMITKUSTE
Credits: Figures 73-74: Courtesy of the AmericanFront and back cover: Photomicrograph of a Wootzsteel prill from the Deccan region ofIndia. The steel isSociety for Testing and Materials; Figures 106, 145,hypereurectoid and cast, and was made in a crucible148, 162: Peter Dorrell, Photography Department,process. Voids appear dark. The pearlite appears in aInstitute of Archaeology, London; Figures 1-8,12-20,variety of colors due to differences in spacing. The26-40,55,198-212: redrawn by Janet Speharwhite needles are cementite; the occasional lighterEnriquez; Figures 198-212: Courtesy of the Interna patches are rich in phosphorus. This crucible steel is ational Copper Research and Development Association;high-quality product of ancient historic significance.Figures 75-80: Dennis Keeley; Cover, Plates 1-20,Color interference tint etched in selenic acid. x420.Figures 9-11, 21-25, 41-54: David A. Scott.Publications Coordinator: Irina Averkieff, GCIEditor: Irina AverkieffTechnical Drawing: Janet Spehar EnriquezDesign: Marquita Stanfield Design, Los Angeles, CaliforniaTypography: FrameMaker / Adobe Garamond and Gill SansPrinting: Tien Wah Press, Ltd. 1991 The J. Paul Getty TrustAll rights reservedPublished in association with Archetype Books which acknowledge a grantfrom the Commission of European CommunitiesPrinted in SingaporeLibraty of Congress Cataloguing-in-Publication DataScott, David A.Metallography and microstructure of ancient and historic metals/David A. Scott.p. cm.Includes bibliographical references and index.ISBN 0-89236-195-6 (pbk.)1. Metallography. 2. Alloys--Metallography. 3. Metallographicspecimens. 4. Art objects--Conservation and restoration.I. Tide.TN690.S34 1991669'.95--dc2091-19484CIP
THE GETrY CONSERVATION INSTITUTEThe Getty Conservation Institute, an operatingprogram of the J. Paul Getty Trust, was createdin 1 982 to address the conservation needs of ourcultural heritage. The Institute conducts world wide, interdisciplinaty professional programs inscientific research, training, and documentation.This is accomplished through a combination ofin-house projects and collaborative ventureswith other organizations in theUSAand abroad.Special activities such as field projects, interna tional conferences, and publications strengthenthe role of the Institute.
TABLE OF CONTENTSForewordPrefaceList of Color Plates and FiguresColor PlatesIXIXXlxvliThe Nature of Metals52The Microstructure of Ancient Metals3Two-phased Materials114The Microstructure of Tin Bronzes255Notes on the Structure of Carbon Steels316Martensite in Low-carbon Steels337The Tempering of Martensite358Structure and Properties of Cast I ron379Corroded Microstructures4310Reflected Polarized Light M icroscopy4911Grain Sizes of Ancient Metals5112Metallography and Ancient Metals5713Metallographic Sampling of Metals6114Mounting and Preparing Specimens6315Recording Results6716Etching and Etching Solutions6917Mounting Resins7518Microhardness Testing77AAppendix: Common Microstructural Shapes79BAppendix: Microstructure of Corroded Metals81CAppendix: Microhardness Values for Different Alloys and Metals82DAppendix: Alloys Used in Antiquity84EAppendix: Terms and Techniques in Ancient Metalworking85FAppendix: Metallographic Studies86GAppendix: Phase Diagrams121Glossary1 37Bibliography1 47Index151
FOREWORDInformation about the structure of materials andtechnology of manufacture of ancient and his toric objects and artifacts can provide insight intotheir date, place of origin, and probable use.Investigations of structure may also be veryimportant for documentation, preservation strat egy, or conservation treatment. For many decadesobjects from a variety of materials and datingfrom prehistoty to the present have been scientif ically studied, many of them by metallographictechniques. Most of the results are scatteredthroughout the international literature, are some times inaccessible, and often not published at all.Frequently the need has been expressed, innational and international meetings, to collectinformation on certain types of objects or classesof materials in one place and to make it availableas a database or publication. This volume is anattempt to provide a measured amount of infor mation regarding the techniques of metallogra phy as they apply to ancient and historic metals.It is illustrated with many examples of differenttypes of microstructure, drawn from David Scott'smany years of experience in this field of study.We hope that the present volume, developedwith the guidance of Dr. Frank Preusser, Associ ate Director, Programs, GCl, will be a usefulbook for students, conservators, conservation sci entists, and workers in the area of metallography,especially those seeking to understand the natureof microstructure as it applies to ancient materi als. The book is the first in a series of referenceworks that the Getty Conservation Institute ispublishing on materials used in conservation andtechnology. The Getty Conservation Instituteand the ] . Paul Getty Museum have beeninvolved collaboratively with this work andpresent this volume as copublishers.Miguel Angel CorzoDirectorThe Getty Conservation InstituteMarina del Rey, California
PREFACEThis book began as a series of laboratory notesof samples for metallographic study. The quanti and the author hopes that in the process of rewrit tative interpretation of alloy phase diagrams hasing and integrating, the original text has been ren not been included here, and in general, mathe dered more accessible. There are many studies ofmatical content has been kept to a minimum.ancient and historic metalwork published in theThe practical information in the text also includesliterature, but it is more difficult to find a generaldetails on etching solutions and short accounts ofaccount of metallographic techniques and anmicrohardness and the grain size of metals. Thereinterpretation of microstructure written primarilyis a lengthy appendix (F) in which examples offor the conservation scientist and conservator.different rypes of alloys and microstructures areThis book attempts to fill this gap by ptoviding agiven, drawn from studies carried out by theguide to the structure of metals. From the mate author. This appendix is not comprehensive, butrials science perspective, it is also useful to exploreit is hoped that the reader will find it interestingthe ways in which alloys have been used inand informative.ancient metalwork.The analytical data that have been presentedThere are many reasons for studying thein the book are quoted without a discussion ofstructure of metals. The proper conservation ofhow the results have been obtained. There areobjects requires or sometimes enables the conser many accounts of analytical methods and tech vator to observe microstructure. Investigativeniques, such as electron microprobe analysis,studies may be necessary in order to assess theatomic absorption spectrophotometry, induc degree of corrosion or embrittlement of an object.tively coupled plasma mass spectrometry, andA new conservation treatment may have implica ray fluorescence analysis, and one or more oftions for the preservation of metallographic struc these techniques are the principal methods byture. Cyril Stanley Smith states that the hierarchywhich the results quoted in the text have beenx of structure can be examined at many differentobtained. It was not the aim of the present text tolevels ofaggregation and that the incorporation ofenter into detail concerning the chemical analysisempirical experience of materials into a theoreti of metals. Similarly, although corrosion and cor cal framework has enabled materials science torosion products are often essential components ofappreciate the effects of structure on propertiesancient metals, there is no detailed discussion ofand even the artistic qualities of materials. It isthe nature of corrosion products given, since tocertainly true that metallographic structuresdo so would add substantially to the length of thethemselves are often visually compelling both in abook. The smelting, casting, and working of met scientific and an artistic sense. Metals are interest als is also not covered in detail by the text,ing materials since their properties can be manip although the glossary does provide some informa ulated in many ways. By combining metals, bytion and common terms used in describing metalsheating and quenching, by making them liquidand metalworking processes.and casting them, or by working them to shapewith a hammer or a lathe, they allow a plasticiryAcknowledgmentsof movement while being shaped and a finaliry ofThe author is very grateful to the staff of theform when that process is completed.The structure of the book should have a wordGetry Conservation Institute PublicationsDepartment for seeing the manuscript throughof explanation here. The approach that has beenfrom editing to printing, in particular to Irinataken is to describe briefly what metals are and toAverkieff for her thoughtful and dedicated edito discuss phase diagrams and the kinds of structuresrial work. Janet Enriquez was responsible forto be found in different and relevant alloys, beforeredrawing the original figures, Dennis Keeleyproceeding to deal with the practical applicationtook the photographs in Chapter 1 1 , and Mar of this knowledge: the sampling and preparationquita Stanfield directed the overall design. Nota-
bly, Frank Preusser, Associate Director forPrograms, and Irina Averkieff, PublicationsCoordinator, must be thanked for their enthusi asm and support.The author is also grateful to Summer SchoolsPress for assistance with the publication of thefirst version of the text.Several of the photomicrographs taken by theauthor would not have been possible without thehelp and assistance provided by those who havegenerously devoted samples or time to the cause.In particular I would like to thank Dr. Nigel See ley, former Head of the Department of Conserva tion and Materials Science, Institute of Archae ology, London, currently Surveyor of Conserva tion, National Trust, London; James Black,International Academic Projects, London; Dr.Rodney Clough, formerly Research Associate,Department of Conservation and Materials Sci ence, London, and former students of theDepartment, Noel Siver, Heather Burns, BobHaber, Dr. Warangkhana Rajpitak, NaylourGhandour, Dr. Abdulrasool Vatandoost Haghighi, and Jane Porter. I would like to givethanks to the following members of the staff atthe Institute of Archaeology: Dr. Warwick Bray,Reader in South American Prehistory; Peter Dor rell, Head of the Photography Department; andStuart Laidlaw, Senior Photographic Technician.At the Getty Conservation Institute I wouldlike to thank, in addition, my secretary RuthFeldman, who has carried out many retyping andreformatting jobs in connection with the prepara tion of the manuscript; Dr. Neville Agnew,Director of Special Projects; and Michael Schill ing, Associate Scientist. From the J. Paul GettyMuseum I am most grateful to Jerry Podany,Head of the Department of Antiquities Conser vation and Linda Strauss, Associate Conservator,Department of Decorative Arts and SculptureConservation.Dr. David A. ScottHead, Museum ServicesThe Getty Conservation Institute
COLOR PLATESANDFIGURESin Ag-Cu.Fig. 39. Cu-Au phase diagram.axe.Plate I. Section from a LurisranFig. 7 . Progressive movement o f andagger handle.edge dislocation.Plate 2. Fragment of corrosion crustFig. 40. Cu-Pb phase diagram.fragment from an Ecuadorian gildedfrom a Chinese cast iron lion.Fig. 8. Dendrite atms.Fig. 9. Polished and unetched viewFig. 41. Cast toggle pin from Iran.copper ceremonial axe.Fig. 71. Section of a corrodedPlate 3. Section from an outdoorof a section through a "Darien"-sryleFig. 42. Chinese cast-bronze incenseFig. 72. Nomograph for grain size.bronze sculpture.Plate 4. Fragment of a brasspectoral from Ancient Colombia.Fig. 73. Typical standard forFig. 10. Polished section of a smallburner.Fig. 43. A small mirror of beta medallion from the La Perousecast frog from the Tairona area ofquenched bronze from Sumatra.of steel.shipwreck off the coast of Australia.Colombia.Fig. 44. High-tin bronze mirrorFig. 74. Typical standard forestimating the (austenitic) grain sizeestimating the (austenitic) grain sizePlate 5. Roman mitror fromFig. Ila-f. Some microstructuralfrom Java.Canterbury.features in solid solution FCCFig. 45. Cast high-tin leaded bronzeof annealed nonferrous materialsPlate 6. Corroded section of aRoman incense burner.metals.of 22% tin,6% lead,and 72%such as brass,bronze,and nickelFig. 12. Relationship between single phase strucrures in FCC metals.copper.Fig. 46. Laborarory quenched alloysilver.Plate 7. Cast iron fragment from19th-century scales.Plate 8. Section from a high-tinFig. 13. Section through copper alloyFig. 76. Grinding mounted samples.axe from Iran showing twinnedof 24% tin,76% copper.Figs. 47-50. Japanese sword bladebronze vessel from Thailand.grains.fragment.Fig. 78. Sample storage.Plate 9. Section from a Greek Hermof about 120Fig. 14. Twinned grains of gold copper alloy sheet.Fig. 15. Twin planes in Indian zincFig. 51. Partially WidmanstattenFig. 79. Examination by polarizedsteel.light microscopy.Fig. 52. Grain boundary structureFig. 80. Use of inverted stagecowith subgrain features.metallurgical microscope.Fig. 16. Twin planes in zinc.Fig. 53. Grain size of knife edge.Fig. 81. Drawing of an axe showingFig. 17. Twin planes in zinc.Fig. 54. Banded structure of aideal location of sample cuttings.Fig. 18. Phase diagram for the gold silver system.Fig. 19. Eutectic diagram of silver quenched sword blade.Fig. 82. Two samples of mountedFig. 55. Part of the Fe-Fe3C phasewire or rod.diagram.Fig. 83a-c. Holding small samples.Plate 13. Section of a cast ironcopper alloy.Fig. 56. Steel prill from lid of acannonball hom Sandal Castle.Fig. 20. Eutectic-rypeWootz crucible, Deccan area ofIndia.Fig. 84a-d. Embedding smallsamples.B.C.Plate 10. Iranian Iron Age daggerhilt.Plate II. Section of an Islamicinkwell.Plate 12. Section of a corroded castiron cannonball from the Tower ofLondon.111.Plate 14. Section of a high-tin bronzemicrostructures.mirror from Java.Plate 15. Section from a small IndianFig. 21. Dendriticain 60% Ag 40%Fig. 57. Medieval knife blade fromArdingley,Sussex, England.Cu cast alloy.Fig. 75. Mounting small specimens.Fig. 77. Polishing mounted samples.Fig. 85. Shapes of ferrite in low carbon steels.Fig. 86. Common descriptiveWootz ingot.Fig. 22. 60% Ag 40% Cu etched inFig. 58. Photomicrograph of krismicrostructural terms.Plate 16. Section from a Japanesepotassium dichromate.from India.Figs. 87-89. Base silver-copper alloyswotd blade.Fig. 23. 60% Ag 40% Cu cast alloyFigs. 59,60. French cut-steel bead.coin from western India.Plate 17. Late Bronze Age swordillustrating eutectic infill.Fig. 61. Part of the Fe-Fe3C phaseFigs. 90-93. Islamic inlaid inkwellfrom Palestine.Fig. 24. Wootz steel ingot from Indiadiagram for cast iron.cast in a copper-tin-zinc-Iead alloy.Plate 18. Polished and etched sectionFigs. 25a,b.Fig. 62a-f. Flake graphite in castFigs. 94-96. Cast bronze arrowheadof a late medieval Indian zinc coin.microstructures.Plate 19. Section of a small Luristanceremonial axe from Iran.Fig. 26. EutecticPlate 20. Section from inside thebase of a Greek Herm.aand Iron.from Palestine.Figs. 97-99. Palestine bronze sword.Fig. 27. Eutectic and dendrites.Fig. 63. 18th-century cast iron scales.Fig. 64. Cast iron cannonball fromFig. 28. Fibrous structure in workedthe Tower of London.Figs. 101-103. Colombian gold two-phase alloy.Fig. 29. and eutectoid.Fig. 65. Typical variations in thecopper alloy sheet.Fig. !. Close-packed hexagonal unitpreservation of surface detail inFigs. 104,105. Ecuadorian copper cell structure.Fig. 30. Iron-carbon phase diagram.ancient metallic artifacts.alloy nose ornament.Fig. 2. Face-centered cubic unit cell.Fig. 31a-d. Breakdown ofFig. 66. Mounted and polishedFigs. 106-108. Cast arsenical copperaand .aIi 0a grains.Fig. 100. Roman wrought iron.Fig. 3. Body-centered cubic unit cell.Fig. 32. Cementite and pearlite.section through a bronze rodaxe from Ecuador.Fig. 4. Graph of relationshipFig. 33. Copper-tin phase diagram.fragment.Figs. 109, 110. Chinese bronzebetween stress and strain.Fig. 5a, b. Stress and strain relationFig. 34.Fig. 67. Drawing of the cross sectionincense burner.of a bronze rod fragment.Fig. Ill. Thai bronze cast bell.Figs. 112,113. Luristan daggerhandle.Figs. 114, 115. Fragment of a ThaiFig. 35.E peritectic.phase grains.Fig. 36. Copper-zinc phase diagram.Fig. 37. grains in copper-zinc.Fig. 68a-d. Examples of corrosion ofstrain for interstitial materials.Fig. 6. An edge dislocation.Fig. 38. Discontinuous precipitationFigs. 69,70. Luristan ceremonialfor FCC,BCC,and C P H; stress andgold-copper alloys.
bronze container.Figs.116,117. Columbian cast Simlear ornament.Figs. IIS-120. Cast iron cannonballFig. 173. Section of a circularglobular region of pearlite.bracelet from Thailand.Fig. 174. Structure of the circularMurakami's reagent and picral.Fig. 194. White cast iron etched inbracelet from Thailand after etchingFigs. 195,196. Tin ingot fromfrom Sandal Castle.in alcoholic ferric chloride.Cornwall.Figs. 121,122. Bronze Age copperingot from Hampshire, England.Fig. 175. High magnification ofcircular bracelet from Thailandvalue,and hardness of wroughtFigs. 123-125. Roman brass coin.showing redeposited copper,coppercopper-tin alloys.Figs. 126,127. Thai bronzesulfide inclusions, and bronze metal.Fig. 198. Copper-tin system.container fragment.Figs. 128-130. Gold necklace beadfrom Colombia.Fig. 176. Section through a RomanFig. 199. Part of the copper-tinbronze bowl,lightly etched indiagram under different conditions.alcoholic ferric chloride.Fig. 200. Copper-arsenic system.Fig. 177. Early medieval brass sheetetched in alcoholic ferric chlorideFig. 201. Copper-lead binary system.Fig. 202. Copper-iron binary system.and potassium dichromate.Fig. 17S. Recrystallized and heavilyFig. 203. Copper-gold binarysystem.Figs. 136,137. Iron knife.Fig. 138. Roman copper alloy coin.Figs. 139,140. Roman iron nail.worked grain structure of brass stud.Fig. 204. Copper-antimony binarysystem.Romano-Greek iron arrowhead.Fig. 205. Copper-silver binaryFigs. 141-144. Native copper fromFig. 180. Unusual corrosion patternsystem.the Great Lakes region in NorthAmerica.through Byzantine bronze blade.Fig. 206. Copper-nickel binaryFig. lSI. Heavily etched view ofsystem.Figs. 145-147. Head of a roggle pinByzantine leaf-shaped blade.Fig. 182. Corroded iron knife bladefrom medieval Britain.Fig. 207. Copper-zinc binary system.Figs. 131-133. Gold alloy nail andgold ear spool.Figs. 134,135. Tang and bladesectlon.from Iran.Figs. 148-151. Javanese iron blade.Fig. 179. Microstructure ofFig. 197. Tensile properties, impactFig. 208. Iron-carbon system.Fig. 209 a. Lead-tin system(pewters). b. Gold-silver system.Figs. 152, 153. Bronze axe fragmentFig. 183. Iron knife blade showing afrom Iran.weld where different pieces of ironhave been joined togerher.Fig. 184. Low-carbon steel area ofFig. 210. Copper-silver-gold ternaryliquidus.medieval iron knife blade.Fig. IS5. Section of panpipes etchedsolidus.Figs. 154,155. Laboratory cast60:40 brass.Figs. 156-159. Gilded silver earringfrom Jordan.Figs. 160, 161. Fragment of a brassin cyanide/persulfate.medallion from AustralianFig. IS6. Fragment of Byzantine ironshipwreck.dagger blade showing part of theFigs. 162-164. Fragment of a smallSiml ear ornament.edge.Fig. 187. Overall view of the RomanFig. 165. Roman mirror fragment.coin of Victoren us etched inFig. 166. Roman bronze figurine.alcoholic ferric chloride.Fig. 167. Roman btonzeFig. lS8. Grain structure of themicrostructure.
entists, and workers in the area of metallography, especially those seeking to understand the nature of microstructure as it applies to ancient materi als. The book is the first in a series of reference works that the Getty Conservation Institute is publishing on materials used in conservation and technology. The Getty Conservation Institute
1. Study of Equipment Manual of Replica Metallography 2. Study of PT Techniques 3. Practical Work 2. REPLICA METALLOGRAPHY Surface Replication is a well developed electron microscopy sample preparation technique that can be used to conduct in situ measurements of the microstructure of components. The in situ
4/13/2021 Metallography with Color and Contrast Learn & Share Leica Microsystems allography-with-color-and .
metallography microstructures (Zones A and B) were observed at 400X. The 500X magnification for traditional samples was chosen because it was the nearest to the magnification of the CIDESI’s portable microscope (400X). Details of the sample preparation in the laboratory and the sample preparation for in situ metallography can be .
The use of metallography for examination of radioactive specimens is considerably more complicated than for exami nation of ordinary materials, but improveiaents in hot laboratory techniques are making it possible to obtain much valuable information. This report describes the KAPL procedtire for performing raaote metallography and discusses
METALLOGRAPHY GUIDE FOR XEROX 4008 ALUMINUM WIRE White Paper - Metallography Guide for Xerox 4008 Aluminum Wire 7 of 9 Figure 6. 4008-F specimen etched using Weck's reagent. Grain boundaries are less clear than when examined in the T6 condition (Figure 5). Figure 7. 4008-T6 specimen etched using NaOH. KOH yields a similar appearance.
Conventional metallographic techniques causes further damage to the component under investigation. In-situ metallography is an . Etching Ell the polished mirror like surface with suitable etchant and cleaning i 140. S. DAS 5. Finally observing the microstructure under an optical or electron Microscope.
based on microstructure study. It is also presents the microstructure changes and properties of 106720 service hour exposed boiler tube in a 120 MW boiler of a thermal power plant. Keywords-service exposed boiler tubes, microstructure, remaining life analysis, creep. I. INTRODUCTION In recent years, from oil refinery to
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