ASTM E407-2007e1 0000 Standard Practice for Microetching Metals and Alloys《金属和合金微蚀的标准操作规程》.pdf

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1、Designation: E407 071Standard Practice forMicroetching Metals and Alloys1This standard is issued under the fixed designation E407; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses i

2、ndicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1NOTETable 2 was editorially corrected in May 2011.1. Scope1.1 This practice covers chemi

3、cal solutions and proceduresto be used in etching metals and alloys for microscopicexamination. Safety precautions and miscellaneous informa-tion are also included.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the

4、 user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificcautionary statements, see 6.1 and Table 2.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE7 Terminology

5、Relating to MetallographyE2014 Guide on Metallographic Laboratory Safety3. Terminology3.1 Definitions:3.1.1 For definition of terms used in this standard, seeTerminology E7.3.2 Definitions of Terms Specific to This Standard:3.2.1 tint etchan immersion etchant that produces colorcontrast, often selec

6、tive to a particular constituent in themicrostructure, due to a thin oxide, sulfide, molybdate, chro-mate or elemental selenium film on the polished surface thatreveals the structure due to variations in light interferenceeffects as a function of the film thickness (also called a 88stainetch”).3.2.2

7、 vapor-deposition interference layer method a tech-nique for producing enhanced contrast between microstructuralconstituents, usually in color, by thin films formed by vacuumdeposition of a dielectric compound (such as ZnTe, ZnSe,TiO2, ZnS or ZnO) with a known index of refraction, generallydue to li

8、ght interference effects (also known as the “Pepperhoffmethod”).4. Summary of Practice4.1 Table 1 is an alphabetical listing of the metals (includ-ing rare earths) and their alloys for which etching informationis available. For each metal and alloy, one or more etchantnumbers and their corresponding

9、 use is indicated. Alloys arelisted as a group or series when one or more etchants arecommon to the group or series. Specific alloys are listed onlywhen necessary. When more than one etchant number is givenfor a particular use, they are usually given in order ofpreference. The numbers of electrolyti

10、c etchants are italicizedto differentiate them from nonelectrolytic etchants.4.2 Table 2 is a numerical listing of all the etchants refer-enced in Table 1and includes the composition and generalprocedure to be followed for each etchant.4.3 To use the tables, look up the metal or alloy of interestin

11、Table 1 and note the etchant numbers corresponding to theresults desired. The etchant composition and procedure is thenlocated in Table 2corresponding to the etchant number.4.4 If the common name of an etchant is known (Marbles,Vilellas, etc.), and it is desired to know the composition,Table 3contai

12、ns an alphabetical listing of etchant names, eachcoded with a number corresponding to the etchant compositiongiven in Table 2.1This practice is under the jurisdiction of ASTM Committee E04 on Metallog-raphy and is the direct responsibility of Subcommittee E04.01 on SpecimenPreparation.Current editio

13、n approved May 1, 2007. Published May 2007. Originallyapproved in 1999. Last previous edition approved in 1999 as E40799 DOI:10.1520/E0407-07.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards vol

14、ume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 This practice lists recommended methods and solutionsfor the etching of speci

15、mens for metallographic examination.Solutions are listed to highlight phases present in most majoralloy systems.6. Safety Precautions6.1 Before using or mixing any chemicals, all product labelsand pertinent Material Safety Data Sheets (MSDS) should beread and understood concerning all of the hazards

16、 and safetyprecautions to be observed. Users should be aware of the typeof hazards involved in the use of all chemicals used, includingthose hazards that are immediate, long-term, visible, invisible,and with or without odors. See Guide E2014 on MetallographicLaboratory Safety for additional informat

17、ion on; ChemicalSafety, Electrolytic Polishing/Etching and LaboratoryVentilation/Fume Hoods.6.1.1 Consult the product labels and MSDSs for recommen-dations concerning proper protective clothing.6.1.2 All chemicals are potentially dangerous. All personsusing any etchants should be thoroughly familiar

18、 with all of thechemicals involved and the proper procedure for handling,mixing, and disposing of each chemical, as well as anycombinations of those chemicals. This includes being familiarwith the federal, state, and local regulations governing thehandling, storage, and disposal of these chemical et

19、chants.6.2 Some basic suggestions for the handling and disposingof etchants and their ingredients are as follows:6.2.1 When pouring, mixing, or etching, always use theproper protective equipment, (glasses, gloves, apron, etc.) andit is strongly recommended to always work under a certifiedand tested

20、fume hood. This is imperative with etchants thatgive off noxious odors or toxic vapors that may accumulate orbecome explosive. In particular, note that solutions containingperchloric acid must be used in an exclusive hood equippedwith a wash down feature to avoid accumulation of explosiveperchlorate

21、s. See Guide E 2014E2014 on MetallographicLaboratory Safety for additional information on safety precau-tions for electrolytes containing perchloric acid6.2.2 No single type of glove will protect against allpossible hazards. Therefore, a glove must be carefully selectedand used to ensure that it wil

22、l provide the needed protection forthe specific etchant being used. In some instances it may benecessary to wear more than one pair of gloves to provideproper protection. Information describing the appropriate glovemay be obtained by consulting the MSDS for the chemicalbeing used. If that does not p

23、rovide enough detailed informa-tion, contact the chemical manufacturer directly. Additionally,one can contact the glove manufacturer or, if available, consultthe manufacturers glove chart. If the chemical is not listed or ifchemical mixtures are being used, contact the glove manufac-turer for a reco

24、mmendation.6.2.3 Use proper devices (glass or plastic) for weighing,mixing, containing, and storage of solutions. A number ofetchants generate fumes or vapors and should only be stored inproperly vented containers. Storage of fuming etchants insealed or non-vented containers may create an explosionh

25、azard.6.2.4 When mixing etchants, always add reagents to thesolvent unless specific instructions indicate otherwise.6.2.5 When etching, always avoid direct physical contactwith the etchant and specimen; use devices such as tongs tohold the specimen (and tufts of cotton, if used).6.2.6 Methanol is a

26、cumulative poison hazard. Where etha-nol or methanol, or both are listed as alternates, ethanol is thepreferred solvent. Methanol should be used in a properlydesigned chemical fume hood.6.2.7 When working with HF always be sure to wear theappropriate gloves, eye protection and apron. Buying HF at th

27、elowest useable concentration will significantly reduce risk.Additionally, it is recommended that a calcium gluconatecream or other appropriate HF neutralizing agent be availablefor use if direct skin contact of the etchant occurs.6.2.8 The EPA states that human studies have clearlyestablished that

28、inhaled chromium (VI) is a human carcinogen,resulting in an increased risk of lung cancer. Animal studieshave shown chromium (VI) to cause lung tumors via inhalationexposure. Therefore, when working with Cr(VI) compoundssuch as K2Cr2O7and CrO3always use a certified and testedfume hood. Additional in

29、formation can be obtained at the EPAwebsite3.6.2.9 For safety in transportation, picric acid is distributedby the manufacturer wet with greater than 30% water. Caremust be taken to keep it moist because dry picric acid is shocksensitive and highly explosive especially when it is combinedwith metals

30、such as copper, lead, zinc, and iron. It will alsoreact with alkaline materials including plaster and concrete toform explosive compounds. It should be purchased in smallquantities suitable for use in six to twelve months and checkedperiodically for lack of hydration. Distilled water may beadded to

31、maintain hydration, It must only be stored in plastic orglass bottles with nonmetallic lids. If dried particles are notedon or near the lid, submerge the bottle in water to re-hydratethem before opening. It is recommended that any bottle ofpicric acid that appears dry or is of unknown vintage not be

32、opened and that proper emergency personnel be notified.6.2.10 Wipe up or flush any and all spills, no matter howminute in nature.6.2.11 Properly dispose of all solutions that are not identi-fied by composition and concentration.6.2.12 Store, handle and dispose of chemicals according tothe manufactur

33、ers recommendations. Observe printed cau-tions on reagent bottles.6.2.13 Information pertaining to the toxicity, hazards, andworking precautions of the chemicals, solvents, acids, bases,etc. being used (such as material safety data sheets, MSDS)should be available for rapid consultation.Aselection o

34、f usefulbooks on this subject is given in Refs. (1-11)4.6.2.14 Facilities which routinely use chemical etchantsshould have an employee safety training program to insure theemployees have the knowledge to properly handle chemicaletchants.3http:/www.epa.gov/ttn/atw/hlthef/chromium.html4The boldface nu

35、mbers in parentheses refer to the list of references at the endof this standard.E407 07126.2.15 When working with etchants always know where thenearest safety shower, eye-wash station, and emergency tele-phone are located.7. Miscellaneous Information7.1 If you know the trade name of an alloy and nee

36、d toknow the composition to facilitate the use of Table 1, refer toa compilation such as Ref (12).7.2 Reagent grade chemicals shall be used for all etchants.Unless otherwise indicated, it is intended that all reagentsconform to specifications of the Committee on AnalyticalReagents of the American Ch

37、emical Society where suchspecifications are available. Other grades, such as United StatesPharmacopeia (USP), may be used, provided it is first ascer-tained that the reagent is of sufficiently high purity to permit itsuse without detrimental effect.7.2.1 Unless otherwise indicated, references to wat

38、er shallbe understood to mean reagent water as defined by Type IV ofspecification D1193. Experience has shown that the quality oftap water varies significantly and can adversely affect someetchants.7.3 Methanol is usually available only as absolute methanol.When using this alcohol it is imperative t

39、hat approximately 5volume % of water is added whenever an etchant compositioncalls for 95 % methanol. Some of these etchants will not workat all if water is not present.7.4 For conversion of small liquid measurements, there areapproximately 20 drops/mL.7.5 Etching should be carried out on a freshly

40、polishedspecimen.7.6 Gentle agitation of the specimen or solution duringimmersion etching will result in a more uniform etch.7.7 The etching times given are only suggested startingranges and not absolute limits.7.8 In electrolytic etching, d-c current is implied unlessindicated otherwise.7.9 Agood e

41、conomical source of d-c current for small scaleelectrolytic etching is the standard 6-V lantern battery.7.10 In electrolytic etching, the specimen is the anodeunless indicated otherwise.7.11 Do not overlook the possibility of multiple etchingwith more than one solution in order to fully develop thes

42、tructure of the specimen.7.12 Microscope objectives can be ruined by exposure tohydrofluoric acid fumes from etchant residue inadvertently lefton the specimen. This problem is very common when thespecimen or mounting media contain porosity and when themounting material (such as Bakelite) does not bo

43、nd tightly tothe specimen resulting in seepage along the edges of thespecimen. In all cases, extreme care should be taken to removeall traces of the etchant by thorough washing and completedrying of the specimen before placing it on the microscopestage.7.13 Tint etchants (13, 14-16) are always used

44、by immer-sion, never by swabbing, as this would inhibit film formation.An extremely high quality polish is required as tint etchantswill reveal remaining polishing damage even if it is not visiblewith bright field illumination.After polishing, the surface mustbe carefully cleaned. Use a polyethylene

45、 beaker to contain theetchant if it contains fluorine ions (for example, etchantscontaining ammonium bifluoride, NH4FHF). The specimen isplaced in the solution using tongs, polished face up. Gentlyagitate the solution while observing the polished surface. Aftercoloration begins, allow the solution t

46、o settle and remainmotionless. Remove the specimen from the etchant when thesurface is colored violet, rinse and dry. A light pre-etch with ageneral-purpose chemical etchant may lead to sharper delinea-tion of the structure after tint etching.7.14 Specimens should be carefully cleaned before use of

47、avapor-deposition interference film (“Pepperhoff”) method (13,14-17). A light pre-etch, or a slight amount of polishing relief,may lead to sharper delination of the constituents after vapordeposition. The deposition is conducted inside a vacuumevaporator of the type used to prepare replicas for elec

48、tronmicroscopy. One or several small lumps of a suitable dielectriccompound with the desired index of refraction is heated undera vacuum until it evaporates.Avacuum level of 1.3 to 0.013 Pa(103to 105mm Hg) is adequate and the polished surfaceshould be about 1015 cm beneath the device that holds thed

49、ielectric compound. Slowly evaporate the lumps and observethe surface of the specimen. It may be helpful to place thespecimen on a small piece of white paper.As the film thicknessincreases, the surface (and the paper) will become colored withthe color sequence changing in the order yellow, green, red,purple, violet, blue, silvery blue. Stop the evaporation when thecolor is purple to violet, although in some cases, thinner filmswith green or red colors have produced good results.7.15 Metals Handbook (18) provides additional advice onetching solutions and techniques for va