ASTM E407-2007(2015)e1 3695 Standard Practice for Microetching Metals and Alloys《金属和合金微蚀的标准实施规程》.pdf

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1、Designation: E407 07 (Reapproved 2015)1Standard 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 numbe

2、r in parentheses indicates 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 U.S. Department of Defense.1NOTEOriginally approved date was editorially corrected to 1970 in

3、 footnote 1.1. Scope1.1 This practice covers chemical 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, assoc

4、iated with its use. It is theresponsibility of the 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:2D1

5、193 Specification for Reagent WaterE7 Terminology 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 immersio

6、n etchant that produces colorcontrast, often selective 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

7、 film thickness (also called a stainetch”).3.2.2 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

8、 a known index of refraction, generallydue to light 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, on

9、e or more etchantnumbers and their corresponding 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 i

10、n order ofpreference. The numbers of electrolytic 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 t

11、ables, look up the metal or alloy of interestin 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

12、is desired to know the composition,Table 3contains an alphabetical listing of etchant names, eachcoded with a number corresponding to the etchant compositiongiven in Table 2.5. Significance and Use5.1 This practice lists recommended methods and solutionsfor the etching of specimens for metallographi

13、c 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 be1This practice is under the jurisdiction of ASTM Committee E04 on Metal

14、log-raphy and is the direct responsibility of Subcommittee E04.01 on SpecimenPreparation.Current edition approved June 1, 2015. Published September 2015. Originallyapproved in 1970. Last previous edition approved in 2007 as E407071. DOI:10.1520/E0407-07R15E01.2For referenced ASTM standards, visit th

15、e ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. U

16、nited States1read and understood concerning all of the hazards 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 E2

17、014 on MetallographicLaboratory Safety for additional information 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 dangerou

18、s. All personsusing any etchants should be thoroughly familiar 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 gov

19、erning thehandling, storage, and disposal of these chemical etchants.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 st

20、rongly recommended to always work under a certifiedand tested 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 w

21、ash down feature to avoid accumulation of explosiveperchlorates. See Guide E2014 on Metallographic LaboratorySafety for additional information on safety precautions forelectrolytes containing perchloric acid6.2.2 No single type of glove will protect against allpossible hazards. Therefore, a glove mu

22、st be carefully selectedand used to ensure that it will 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 t

23、he MSDS for the chemicalbeing used. If that does not provide enough detailedinformation, contact the chemical manufacturer directly.Additionally, one can contact the glove manufacturer or, ifavailable, consult the manufacturers glove chart. If the chemi-cal is not listed or if chemical mixtures are

24、being used, contactthe glove manufacturer for a recommendation.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 inseal

25、ed or non-vented containers may create an explosionhazard.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

26、 (and tufts of cotton, if used).6.2.6 Methanol is a 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 theappropria

27、te gloves, eye protection and apron. Buying HF at thelowest 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 sta

28、tes that human studies have clearlyestablished that 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 CrO3alway

29、s use a certified and testedfume hood. Additional information 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

30、explosive especially when it is combinedwith metals 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 fo

31、r lack of hydration. Distilled water may beadded to 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 a

32、cid that appears dry or is of unknown vintage not beopened 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

33、 and dispose of chemicals according tothe manufacturers 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)sho

34、uld be available for rapid consultation.Aselection of 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.6.2.15 When

35、 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 need toknow the composition to facilitate the use of Table 1, refer toa compilation such as Ref (12).7.

36、2 Reagent grade chemicals shall be used for all etchants.Unless otherwise indicated, it is intended that all reagents3http:/www.epa.gov/ttn/atw/hlthef/chromium.html4The boldface numbers in parentheses refer to the list of references at the endof this standard.E407 07 (2015)12conform to specification

37、s of the Committee on AnalyticalReagents of the American Chemical 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

38、 effect.7.2.1 Unless otherwise indicated, references to water 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 a

39、bsolute methanol.When using this alcohol it is imperative that 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

40、20 drops/mL.7.5 Etching should be carried out on a freshly 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

41、-c current is implied unlessindicated otherwise.7.9 Agood economical 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 etchin

42、gwith more than one solution in order to fully develop thestructure 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 a

43、nd when themounting material (such as Bakelite) does not bond 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 micr

44、oscopestage.7.13 Tint etchants (13, 14-16) are always used byimmersion, never by swabbing, as this would inhibit filmformation. An extremely high quality polish is required as tintetchants will reveal remaining polishing damage even if it isnot visible with bright field illumination. After polishing

45、, thesurface must be carefully cleaned. Use a polyethylene beakerto contain the etchant if it contains fluorine ions (for example,etchants containing ammonium bifluoride, NH4FHF). Thespecimen is placed in the solution using tongs, polished faceup. Gently agitate the solution while observing the poli

46、shedsurface.After coloration begins, allow the solution to settle andremain motionless. Remove the specimen from the etchantwhen the surface is colored violet, rinse and dry. A lightpre-etch with a general-purpose chemical etchant may lead tosharper delineation of the structure after tint etching.7.

47、14 Specimens should be carefully cleaned before use of 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 vacuume

48、vaporator of the type used to prepare replicas for electronmicroscopy. 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 surfacesho

49、uld be about 1015 cm beneath the device that holds thedielectric 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 a