1、Designation: E1829 14Standard Guide forHandling Specimens Prior to Surface Analysis1This standard is issued under the fixed designation E1829; 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 p
2、arentheses 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 Auger
3、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-en
4、ergy electron diffraction, and electron energy lossspectroscopy, where specimen handling can influence surface-sensitive measurements.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to esta
5、blish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E1078 Guide for Specimen Preparation and Mounting inSurface Analysis2.2 ISO Standards:3ISO 18115-1 Surface chemical analysisVocabularyPart
6、1: General terms and terms used in spectroscopyISO 18115-2 Surface chemical analysisVocabularyPart2: Terms used in scanning-probe microscopy3. Terminology3.1 DefinitionsFor definitions of surface analysis termsused in this guide, see ISO 18115-1 and ISO 18115-2.4. Significance and Use4.1 Proper hand
7、ling and preparation of specimens is par-ticularly 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
8、 the state of the surface so that analysis remainsrepresentative 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).44.3 This guide descri
9、bes methods to minimize the effects ofspecimen 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 infor
10、mation, only broad guidelines andgeneral examples 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
11、 specific problem to be solved orinformation needed, and the particular specimen preparation orhandling procedures required. The surface analyst also isreferred to Guide E1078 that discusses additional proceduresfor preparing, mounting, and analysis of specimens.5. General Requirements5.1 The degree
12、 of cleanliness required by surface-sensitiveanalytical 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 transpo
13、rted to the analyst in acontainer that does not come into direct contact with thesurface of interest.1This 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 Photoelectron Spectrosco
14、py.Current edition approved Oct. 1, 2014. Published November 2014. Originallyapproved in 1996. Last previous edition approved in 2009 as E1829 09. DOI:10.1520/E1829-14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
15、 Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, CP 56, CH-1211 Geneva 20, Switzerland, http:/www.iso.org.4The boldface numbers in parentheses refe
16、r to a list of references at the end ofthis standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.4 In most cases, the analysis will be performed on the “asreceived” specimen. Surface contamination or atmosphericadsorbates are no
17、t usually removed because of the importanceof analyzing an unaltered surface and as these are often theregions of interest. Care must then be taken in handling thespecimen to ensure that no outside agents come in contact withthe surface to be investigated. These agents include: solvents orcleaning s
18、olutions, 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 requirements for a specificspecimen, they should consult the analyst.5.5 In some cases (for e
19、xample, 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 because inhomgeneities are often present. It is recom-mended that this choice be made
20、 in consultation with anexperienced analyst.5.6 Numerous methods exist for the mounting of a specimenin preparation for analysis. Refer to Guide E1078.5.7 Hazardous MaterialsSpecial caution shall be exer-cised with specimens containing potential toxins or otherhazardous materials. Whenever possible,
21、 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 sought. The list in AppendixX1 describes types of specimens by their increasing sen
22、sitivityto 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 HistoryThe history of a specimen can influence thehandling of its surface. For example
23、, 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 becomes toxic.6.3 Specimens Previously Examined by Other AnalyticalTechniquesIt is best
24、 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 specimens analyzed by electron microscopy mayhave been coated to reduce charging. This c
25、oating 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 the surface analysis work first, then theanalysis should be done on a different, bu
26、t 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 surfaces orinterfaces. The degree of care that must to be taken dependsupon the type
27、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 depth (depthprofile) or at a buried interface; and (Type C) information thatwill req
28、uire 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 preparation andpackaging. Ideally, nothing should be allowed to contact thesurface of in
29、terest. 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, multilayers,metal contact layers on semiconductors, coatings, dopantprofiles, and the c
30、hemical 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. In thisclass, the information sought comes from a layer below theoutermost surface an
31、d 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 specimens include those that require prepara-tion by the analyst and includes specim
32、ens 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 (as happens with lapping) or disassembled. Few specialprecautions are needed for sampl
33、es 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 foranalysis. Nonetheless, care should still be taken to not con-taminate the specimen.
34、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 analysis by marking up a drawingor a photograph. If necessary, a scribe or permanen
35、t 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 surface of interest, eitherby hand or with a tool. Do not “protect” the surface of inter
36、estby 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 Contamination7.1 An unprotected hand must never handle specimens,even when the skin will
37、not touch the surface of interest.Fingerprints and hand creams contain mobile species that maymigrate and contaminate the surface of interest.E1829 1427.2 Handling of specimens only should be done with cleantools to ensure that the specimen surface is not altered prior toanalysis. Tools should be ma
38、de 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 use. Nonmagnetic tools should be used if the specimenis susceptible to magne
39、tic fields. Tools should never unneces-sarily touch the specimen surface.7.3 Although gloves and wiping materials are sometimesused to handle specimens, it is likely that their use will resultin some contamination. Care should be taken to avoid con-tamination by talc, silicone compounds, and other m
40、aterialsthat 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 specimen using a compressed gas source(for example, to remove particulates) is likely to
41、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 recommended.7.5 Some common packaging materials (certain brands ofaluminum foil, certain
42、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 packagingmaterial is not in direct intimate contact with the specimenregion of interest. Pa
43、per 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 should select oneof the methods in the list in Appendix X2.8. Specimen Storage and
44、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 become contaminated quickly to the depth ana-lyzed by AES, XPS, SIMS, and other surface
45、 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 volatile species(for example, plasticizers) may be emitted from suchcontainers, fur
46、ther contaminating the surface. Preferably, thesurface to be analyzed should not contact the container or anyother object. Glass jars with an inside diameter slightly largerthan the width of a specimen can hold a specimen withoutcontact with the surface. When contact with the surface isunavoidable,
47、wrapping in clean, pre-analyzed aluminum foilmay be satisfactory. For semiconductor samples, standardwafer carriers are generally adequate.8.1.2.2 Containers, such as glove boxes, vacuum chambers,and desiccators may be excellent choices for storage ofspecimens. A vacuum desiccator may be preferable
48、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 vessels are availablefor shipping air-sensitive specimens between laboratories.8.1.3 Temp
49、erature and HumidityPossible temperature andhumidity effects should be considered when storing or shippingspecimens. Most detrimental effects result from elevated tem-peratures. Additionally, low specimen temperatures 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
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