ASTM E1829-2009 Standard Guide for Handling Specimens Prior to Surface Analysis《先于表面分析的样品处置标准指南》.pdf

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1、Designation: E 1829 09Standard Guide forHandling Specimens Prior to Surface Analysis1This standard is issued under the fixed designation E 1829; 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

2、 parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This guide covers specimen handling and preparationprior to surface analysis and applies to the following surfaceanalysis disciplines:1.1.1 Auge

3、r electron spectroscopy (AES),1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA),and1.1.3 Secondary ion mass spectrometry (SIMS).1.1.4 Although primarily written for AES, XPS, and SIMS,these methods may also apply to many surface-sensitiveanalysis methods, such as ion scattering spectrometry, low-

4、energy electron diffraction, and electron energy loss spectros-copy, where specimen handling can influence surface-sensitivemeasurements.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to a

5、ddress all of thesafety concerns, if any, associated 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.2. Referenced Documents2.1 ASTM Standards:2E 673 Termi

6、nology Relating to Surface AnalysisE 1078 Guide for Specimen Preparation and Mounting inSurface Analysis3. Terminology3.1 DefinitionsFor definitions of surface analysis termsused in this guide, see Terminology E 673.4. Significance and Use4.1 Proper handling and preparation of specimens is par-ticul

7、arly critical for analysis. Improper handling of specimenscan result in alteration of the surface composition and unreli-able data. Specimens should be handled carefully so as to avoidthe introduction of spurious contaminants. The goal must be topreserve the state of the surface so that analysis rem

8、ainsrepresentative of the original subject.4.2 AES, XPS, and SIMS are sensitive to surface layers thatare typically a few nanometres thick. Such thin layers can besubject to severe perturbations from improper specimen han-dling (1).34.3 This guide describes methods to minimize the effects ofspecimen

9、 handling on the results obtained using surface-sensitive analytical techniques. It is intended for the specimenowner or the purchaser of surface analytical services and thesurface analyst. Because of the wide range of types ofspecimens and desired information, only broad guidelines andgeneral examp

10、les are presented here. The optimum handlingprocedures will be dependent on the particular specimen andthe needed information. It is recommended that the specimensupplier consult the surface analyst as soon as possible withregard to specimen history, the specific problem to be solved orinformation n

11、eeded, and the particular specimen preparation orhandling procedures required. The surface analyst also isreferred to Guide E 1078 that discusses additional proceduresfor preparing, mounting, and analysis of specimens.5. General Requirements5.1 The degree of cleanliness required by surface-sensitive

12、analytical techniques often is much greater than for other formsof analysis.5.2 Specimens must never be in contact with the bare hand.Handling of the surface to be analyzed should be eliminated orminimized whenever possible.5.3 Specimens should be transported to the analyst in acontainer that does n

13、ot come into direct contact with thesurface of interest.5.4 In most cases, the analysis will be performed on the “asreceived” specimen. Surface contamination or atmosphericadsorbates are not usually removed because of the importanceof analyzing an unaltered surface and as these are often theregions

14、of interest. Care must then be taken in the handling thespecimen to ensure that no outside agents come in contact with1This guide is under the jurisdiction of ASTM Committee E42 on SurfaceAnalysis and is the direct responsibility of Subcommittee E42.03 on Auger ElectronSpectroscopy and X-Ray Photoel

15、ectron Spectroscopy.Current edition approved May 1, 2009. Published June 2009. Originallyapproved in 1996. Last previous edition approved in 2002 as E 1829 02.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of

16、ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The boldface numbers in parentheses refer to a list of references at the end ofthis standard.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United

17、States.the surface to be investigated. These agents include: solvents orcleaning solutions, gases (including compressed air) or vapors,metals, tissue or other wrapping materials, tape, cloth, tools,packing materials, or the walls of containers. If the specimensupplier is uncertain of the requirement

18、s for a specific speci-men, they should consult the analyst.5.5 In some cases (for example, for a large specimen), itmay be necessary to take a representative sample from thespecimen. Selection of a smaller sample from a larger speci-men should be done while considering the information beingsought b

19、ecause inhomgeneities are often present. It is recom-mended that this choice be made in consultation with anexperienced analyst.5.6 Numerous methods exist for the mounting of a specimenin preparation for analysis. Refer to Guide E 1078.5.7 Hazardous MaterialsSpecial caution shall be exer-cised with

20、specimens containing potential toxins or otherhazardous materials. Whenever possible chemical hazard datasheets should be supplied with the specimen.5.8 The severity of the requirement for specimen handlingvaries dramatically with the condition of the surface and thelocation of the information being

21、 sought. The list in AppendixX1 describes types of specimens by their increasing sensitivityto handling.6. Specimen Influences6.1 The analyst should be advised of the specimen history,special storage or transport requirements, exposure to possiblecontaminants, and the information being sought.6.2 Hi

22、storyThe history of a specimen can influence thehandling of its surface. For example, a specimen that has beenpreviously exposed to a contaminating environment mayreduce the need for exceptional care if the surface becomes lessreactive. Alternatively, the need for care may increase if thesurface bec

23、omes toxic.6.3 Specimens Previously Examined by Other AnalyticalTechniquesIt is best if surface analysis measurements aremade before the specimen is analyzed by other analyticaltechniques because such specimens may become damaged ormay be exposed to surface contamination. For example,insulating spec

24、imens analyzed by electron microscopy mayhave been coated to reduce charging. This coating renders thespecimens unsuitable for subsequent surface analysis. Expo-sure to an electron beam (for example, in a SEM) also caninduce damage or deposit additional contamination. If it is notpossible to perform

25、 the surface analysis work first, then theanalysis should be done on a different, but nominally identical,specimen or area of the specimen.6.4 Information SoughtSurface chemical analysis can beperformed on a wide range of specimens and can be used toobtain very different types of information about s

26、urfaces orinterfaces. The degree of care that must to be taken dependsupon the type of analysis that is required and the nature of theproblem. The information being sought usually falls into threegeneral categories: (Type A) information on the outermostsurface; (Type B) information as a function of

27、depth (depthprofile) or at a buried interface; and (Type C) information thatwill require subsequent specimen preparation by the analyst.6.4.1 Type A specimens include those to be investigated forsurface contamination, surface stains, and adhesion failures.This category requires the most care in prep

28、aration andpackaging. Ideally, nothing should be allowed to contact thesurface of interest. In practice, it may be necessary to wrap thesamples to avoid damage in transit. (See Appendix X3.)6.4.2 Type B specimens include those that require theinvestigation of thick and thin films, single layers, mul

29、tilayers,metal contact layers on semiconductors, coatings, dopantprofiles, and the chemical and physical properties at aninterface between two dissimilar materials. For this category,the packaging requirements are not as stringent although careshould still be taken to not contaminate the specimen. I

30、n thisclass, the information sought comes from a layer below theoutermost surface and superficial surface contamination is notan issue. With semiconductor samples, care should be taken toavoid particulate contamination of the surface as this candegrade the quality of the depth profiles.6.4.3 Type C

31、specimens include those that require prepara-tion by the analyst and includes specimens for in-situ fracture,metallurgical lapping or polishing, and specimens that are partof a larger assembly. Generally, these specimens must beshaped (for example, for fracture), chemically or mechanicallyaltered (a

32、s happens with lapping) or disassembled. Few specialprecautions are needed for samples that are to be fractured, orundergo further sample preparation by the analyst. For speci-men in a larger assembly or subassembly, it may be preferableto leave the specimen in place and let the analyst remove it fo

33、ranalysis. Nonetheless, care should still be taken to not con-taminate the specimen.6.5 Clearly identify all specimens with a unique name oridentifier. If it is possible to permanently attach this identifier tothe specimen (without disturbing the area of interest), do so.Clearly indicate the area of

34、 analysis by marking up a drawingor a photograph. If necessary, a scribe or permanent ink markercan be used on an area adjacent to the areas of interest. If thereis any doubt as to which side of the specimen is to be analyzed,clearly mark the back of the specimen.6.6 PrecautionsDo not touch the surf

35、ace of interest, eitherby hand or with a tool. Do not “protect” the surface of interestby covering it with tape, contaminated foil or porous wrappingmaterial. Do not use a diamond scribe to mark semiconductors.Fragile specimens should not be mounted onto double-sidedtape.7. Sources of Specimen Conta

36、mination7.1 An unprotected hand must never handle specimens,even when the skin will not touch the surface of interest.Fingerprints and hand creams contain mobile species that maymigrate and contaminate the surface of interest.7.2 Handling of specimens only should be done with cleantools to ensure th

37、at the specimen surface is not altered prior toanalysis. Tools should be made of materials that do not transferto the specimen or introduce spurious contaminants ontosurfaces (for example, nickel tools contaminate silicon). Toolsshould be cleaned regularly in high-purity solvents and driedprior to u

38、se. Nonmagnetic tools should be used if the specimenis susceptible to magnetic fields. Tools should never unneces-sarily touch the specimen surface.E18290927.3 Although gloves and wiping materials are sometimesused to handle specimens, it is likely that their use will resultin some contamination. Ca

39、re should be taken to avoid con-tamination by talc, silicone compounds, and other materialsthat are often found on gloves. “Powder-free” gloves have notalc and may be better suited. The surface to be analyzedshould never be touched by the glove or other tool unlessnecessary.7.4 Blowing on the specim

40、en using a compressed gas source(for example, to remove particulates) is likely to cause con-tamination even when using a noble gas (such as argon orhelium) because of the likelihood that the nozzle or thedelivery line may contain oils, organics or particulates. Blow-ing with the mouth is not recomm

41、ended.7.5 Some common packaging materials (certain brands ofaluminum foil, certain brands of transparent adhesive tape, andcertain brands of polyethylene bags) have silicone (siloxane)coatings. These silicones can migrate across surfaces andcontaminate the specimen of interest even when the packagin

42、gmaterial is not in direct intimate contact with the specimenregion of interest. Paper and cloth packing materials avoidsilicone contamination, but they can also be a source of fibercontamination.7.6 To minimize the potential for contamination of the areato be analyzed during handling, the preparer

43、should select oneof the methods in the list in Appendix X2.8. Specimen Storage and Transfer8.1 Storage:8.1.1 TimeThe longer a specimen is in storage, the morecare must be taken to ensure that the surface to be analyzed hasnot been contaminated. Even in clean laboratory environments,surfaces can beco

44、me contaminated quickly to the depth ana-lyzed by AES, XPS, SIMS, and other surface sensitive analyti-cal techniques.8.1.2 Containers:8.1.2.1 Containers suitable for storage should not transfercontaminants to the specimen by means of particles, liquids,gases, or surface diffusion. Keep in mind that

45、volatile species(for example, plasticizers) may be emitted from such contain-ers, further contaminating the surface. Preferably, the surfaceto be analyzed should not contact the container or any otherobject. Glass jars with an inside diameter slightly larger thanthe width of a specimen can hold a sp

46、ecimen without contactwith the surface. When contact with the surface is unavoidable,wrapping in clean, pre-analyzed aluminum foil may be satis-factory. For semiconductor samples, standard wafer carriers aregenerally adequate.8.1.2.2 Containers, such as glove boxes, vacuum chambers,and desiccators m

47、ay be excellent choices for storage ofspecimens. A vacuum desiccator may be preferable to astandard unit and should be maintained free of grease andmechanical pump oil. Cross contamination between specimensalso may occur if multiple specimens are stored together.8.1.2.3 Commercial vacuum-transfer ve

48、ssels are availablefor shipping air-sensitive specimens between laboratories.8.1.3 Temperature and HumidityPossible temperature andhumidity effects should be considered when storing or shippingspecimens. Most detrimental effects result from elevated tem-peratures. Additionally, low specimen temperat

49、ures can lead tomoisture condensation on the surface.8.2 Transfer:8.2.1 ChambersChambers that allow transfer of speci-mens from a controlled environment to an analytical chamberhave been reported (2-4). Controlled environments could beother vacuum chambers, glove boxes (dry boxes), glove bags,reaction chambers, and so forth, which can be attached directlyto an analytical chamber with the transfer made through apermanent valve. Glove bags can be attached temporarily to ananalytical chamber with transfer of a specimen done byremoval and then replacement of a flange on the anal