ASTM_E_2859_-_11.pdf

Designation:E285911Standard Guide forSize Measurement of Nanoparticles Using Atomic ForceMicroscopy1This standard is issued under the fixed designation E2859;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 indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 The purpose of this document is to provide guidance onthe quantitative application of atomic force microscopy(AFM)to determine the size of nanoparticles2deposited in dry form onflat substrates using height(z-displacement)measurement.Unlike electron microscopy,which provides a two-dimensionalprojection or a two-dimensional image of a sample,AFMprovides a three-dimensional surface profile.While the lateraldimensions are influenced by the shape of the probe,displace-ment measurements can provide the height of nanoparticleswith a high degree of accuracy and precision.If the particlesare assumed to be spherical,the height measurement corre-sponds to the diameter of the particle.In this guide,proceduresare described for dispersing gold nanoparticles on varioussurfaces such that they are suitable for imaging and heightmeasurement via intermittent contact mode AFM.Genericprocedures for AFM calibration and operation to make suchmeasurements are then discussed.Finally,procedures for dataanalysis and reporting are addressed.The nanoparticles used toexemplify these procedures are National Institute of Standardsand Technology(NIST)reference materials containing citrate-stabilized negatively charged gold nanoparticles in an aqueoussolution.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 address 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:3E1617 Practice for Reporting Particle Size CharacterizationDataE2382 Guide to Scanner and Tip Related Artifacts in Scan-ning Tunneling Microscopy and Atomic Force Micros-copyE2456 Terminology Relating to NanotechnologyE2530 Practice for Calibrating the Z-Magnification of anAtomic Force Microscope at Subnanometer DisplacementLevels Using Si(111)Monatomic Steps(Withdrawn2015)4E2587 Practice for Use of Control Charts in StatisticalProcess Control2.2 ISO Standards:5ISO 18115-2 Surface Chemical Analysis-Vocabulary-Part2:Terms Used in Scanning-Probe MicroscopyISO/IEC Guide 98-3:2008 Uncertainty of measurementPart 3:Guide to the Expression of Uncertainty in Mea-surement(GUM:1995)3.Terminology3.1 For definitions pertaining to nanotechnology terms,refer to Terminology E2456.3.2 For definitions pertaining to terms associated withscanning-probe microscopy,including AFM,refer to ISO18115-2.3.3 Definitions of Terms Specific to This Standard:3.3.1 agglomerate,nin nanotechnology,an assembly ofparticles held together by relatively weak forces(for example,Van der Waals or capillary),that may break apart into smallerparticles upon processing,for example.E24563.3.1.1 DiscussionUsing imaging based techniques,suchas AFM,it is generally difficult to differentiate between1This guide is under the jurisdiction of ASTM Committee E56 on Nanotech-nology and is the direct responsibility of Subcommittee E56.02 on Characterization:Physical,Chemical,and Toxicological Properties.Current edition approved Dec.1,2011.Published January 2012.DOI:10.1520/E2859-11.2Having two or three dimensions in the size scale from approximately 1 nm to100 nm as in accordance with Terminology E2456;this definition does not considerfunctionality,which may impact regulatory aspects of nanotechnology,but whichare beyond the scope of this guide.3For referenced ASTM standards,visit the 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.4The last approved version of this historical standard is referenced onwww.astm.org.5Available from International Organization for Standardization(ISO),1,ch.dela Voie-Creuse,CP 56,CH-1211 Geneva 20,Switzerland,http:/www.iso.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 agglomerates formed during the deposition process(that is,artifacts)and agglomerates or aggregates that pre-exist in thetest sample.3.3.2 aggregate,nin nanotechnology,a discrete assem-blage of particles in which the various individual componentsare not easily broken apart,such as in the case of primaryparticles that are strongly bonded together(for example,fused,sintered,or metallically bonded particles).E24563.3.2.1 DiscussionUsing imaging based tec