Compilation of Comparative Information on the Analytical Techniques Discussed in This Volume Main information Tra Article Technique probed Types of solid sample No. typical) (typical) (typical) typical) 5.4 REELS 2 nm 100nm All 3 少 6.1 XRF 10 um mm 0.1% 1 6.2 3nm cm ppb-ppm Trace heavy metals Y 3 3 Y 6.3 PIXE Few um 1004m 10 ppm All 3 71 Few um Fewm ppb All,semicond.usually N 12 N Modulation 1m 1004m ppm All,semicond.usually N 2 3 VASE I um cm Flat thin films N 23 Y FTIR Fewμm 204m Variable All 1 Y 82 Raman Scattering Few um 1μm Variable All N 22 Y 83 HREELS 2nm mm 1% All;flat cond.best Y 33 N Bulk All;not all elements NMR N 33 N 42540 RBS T62μ mm 0.01-10% Y/N 3 2 Y 14m 0.01% Hcontaining Y 3 N 1 nm mm 0.1%-10% All;usually single crystal 3 3 3A 150μm 50ppm-1% All Y 人 3 2 nm I um ppb-ppm All,mostly semicond. Y 3 1 3A 100μm Few All,mostly polymer Y 3 2 Y 10.3 SALI 3A 100nm ppb-ppm All,mostly inorg. 3 3 N
Compilation of Comparative Information on the Analytical Techniques Discussed in This Volume Main information Article Technique No. 5.4 6.1 6.2 6.3 7.1 7.2 7.3 8.1 8.2 8.3 8.4 9.1 9.2 9.3 9.4 10.1 10.2 10.3 VI REELS XRF TXRF PKE Photoluminescence Modulation VASE FTIR Raman Scattering HREELS NMR RBS ERS MEIS ISS Dynamic SIMS static SIMS SALI spectrosmpy 1 Pm lw a a am a a Fewpm a a Fewp a a 2 nm am Bulk a am To 2 pn 1Pn 0 3A 0 0. 1 nm 0 2 nm om a 3A am 3A 100 nm rnm un 100 pn Few Pn 100 pm 20 pm llrm un mm 1oow 100 nrn PPrn - Variable Variable 1% 0.01-10% 0.01% 0.1%-10% 50 ppm-1% PPb-PPm Few % PPb-PPrn All All Trace heavy metals All All, semicond. usually All, semicond. usually Flat thin h All All AU; flat cond. best All; not all elements All H containing All; usually single crystal All All, mostly sernicond. All, mostly polymer AU, mostly inorg. Y- 3N N21Y Y 3 3Y Y 3 3Y N1 2N N2 3N N2 3Y N21Y N2 2Y Y3 3N N3 3N YlN3 2Y Y- 3N Y 3 3N Y- 3Y Y3 1Y Y 3 2Y Y 3 3N
Compilation of Comparative Information on the Analytical Techniques Discu tssed in this volume Main information Types of solid 104 SNMS 1.5 nm 50 ppm Flat 2 00 ppm 3 8g 3 um cm 0.05 ppm Sample forms electrode 22 GDMS 100nm Ppt-ppb Sample forms electrode 3 YYy 10. ICPMS 5山m mm ppt Y I Y 10.9 ICPOES 5 um mm ppb All Y 11Y Bulk Crystalline 3 N 11.2 。Up to mm Flat polymer films N 3 11.3NM Bulk Ppm Trace metals 114 NRA 10-100nm 10m 10-100ppm All:Z<21 3 Y 12.2 mm Fat smooth films N 13Y 12.3 MOKE ··30nm 0.5m Magnetic films N 12N AND SUN 12.4 Adsorption ·Outer atoms Large surface area Y soric Chapter :Numbers refer to usage for anaylsis of solid materials. 1 means Extensive:2means medium;3 means not common. capability:Guide only.Often very material/condition ns not used tor trace components
Compilation of Comparative Information on the Analytical Techniques Discussed in This Volume Depth Width (typical) (typical) (typical) 0, 6. Maill ~nllati~ TkCe Types of solid sample (typical) ArrideTechnique probed probed capability No. 10.4 SNMS . 1.5 nm un 50 PPm Flat conductors Y2 2Y 10.5 LIMS *. 10.6 SSMS 0 10.7 GDMS 0 10.8 ICPMS . 10.9 ICPOES 0 ll.' ;E20ll 5 11.2 ;l;g;v 11.3 NAA 11.4 NRA 2 0 0 C Optical 0 : 12.2 scatternmetry z v) 12.3 MOU P 12.4 Adsorption U . . *. 100nm 2pm 1-100ppm All Y3 2Y 3P cm 0.05 ppm Sample formselde Y - 2Y 5w mm PPt All Y21Y 5P mm PPb All Y 11Y 100 nm cm ppt-ppb Sampleformselecd y 3 2 Y Bulk I Crystalline N- 3 N uptomm - - Flatpolymer films N - 3N Bulk - PPt-PPm Trace metals N2 3Y 10-1OOnm lop 10-lOOppm All: z< 21 Y- 3Y 0 - mm - Flatsmoothfilms N 1 3 Y 30nm 0.5~ - Magnetic films N 12N Outeratoms - - LargesurFacearea Y - 2N v) Notes Tbi table should be uscd as a "quick reference" guide ody. CommnrialZnmMuntcThese m typical costs; large ranges depending on sophistication and accessories: 1 means < $50k 2 means $50-300k; 3 means >$300k. "-" means no mmplcre commercia instrument. Usup: Numbers refer to usage for anaylsis of solid materials. 1 means Extensive; 2 means medium; 3 means not common. Tim capz6iliy: Guide only. Often very material/wnditions dependent. "-" means not used for trace components. !i x % * Measured in transmission. iii v) 0 5 'E! m, -I
Light Microscopy 1.2.1 The light microscope uses the visible or near visible portion of the electromagnetic spectrum;light microscopy is the interpretive use of the light microscope.This technique,which is much older than other characterization instruments,can trace its origin to the 17th century.Modern analytical and characterization methods began about 150 years ago when thin sections of rocks and minerals,and the first polished metal and metal-alloy specimens were prepared and viewed with the intention of correlating their structures with their properties.The technique involves,at its very basic level,the simple,direct visual observation of a sample with white-light resolution to 0.2 um.The morphology,color,opacity,and optical properties are often sufficient to characterize and identify a material. Range of samples Almost unlimited for solids and liquid crystals characterized Destructive Usually nondestructive;sample preparation may involve material removal Quantification Via calibrated eyepiece micrometers and image analysis Detection limits To sub-ng Resolving power 0.2μn with white light Imaging capabilities Yes Main use Direct visual observation;preliminary observation for final characterization,or preparative for other instrumentation Instrument cost $2,500-$50,000 or more Size Pocket to large table
Light Microscopy 1.2.1 The light microscope uses the visible or near visible portion of the electromagnetic spectrum; light microscopy is the interpretive use of the light microscope. This technique, which is much older than other characterization instruments, can trace its origin to the 17th century. Modern analytical and characterization methods began about 150 years ago when thin sections of rocks and minerals, and the first polished metal and metal-alloy specimens were prepared and viewed with the intention of correlating their structures with their properties. The technique involves, at its very basic level, the simple, direct visual observation of a sample with white-light resolution to 0.2 pm. The morphology, color, opacity, and optical properties are often sufficient to characterize and identifl a material. Range of samples characterized Destructive Quantification Detection limits Resolving power Imaging capabilities Main use Instrument cost Size Almost unlimited for solids and liquid crystals Usually nondestructive; sample preparation may involve material removal Via calibrated eyepiece micrometers and image analysis To sub-ng 0.2 pm with white light YeS Direct visual observation; preliminary observation for final characterization, or preparative for other instrumentation $2,500-$50,000 or more Pocket to large table 7
Scanning Electron Microscopy (SEM) 1.2.2 The Scanning Electron Microscope(SEM)is often the first analytical instrument used when a "quick look"at a material is required and the light microscope no ron be n is focused int fine probe and sub quently raster sca over a s nall rectangular area.As the beam interacts with the sample it creates various signals(secondary electrons,inter nal currents,photon emission,etc.),all of which can be appropriately detected. These signals are highly localized to the area directly under the beam.By using these signals to modulate the brightness of a cathode ray tube,which is raster nchronism with the ele s fo a the scre has of a nal mic scopic image but with a much greater depth of field.With ancillary detectors,the instrument is capable of elemental analysis. Main use High magnification imaging and composition (elemental)mapping Destructive No,some electron beam damage Magnification range 10x-300,000x;5000x-100,000x is the typical operating range Beam energy range 500 eV-50 keV;typically,20-30 keV Sample requirements Minimal,occasionally must be coated with a conducting film;must be vacuum compatible Sample size Less than 0.Imm,up to 10 cm or more Lateral resolution 1-50 nm in secondary electron mode Depth sampled Varies from a few nm to a few um,depending upon the accelerating voltage and the mode of analysis Bonding information No Depth profiling Only indirect capabilities Instrument cost s100,000-$300,000 is typical Size goaok3丘x5idkaabemolm INTRODUCTION AND SUMMARIES Chapter 1
Scanning Electron Microscopy (SEM) 1.2.2 The Scanning Electron Microscope (SEM) is often the first analytical instrument used when a "quick look" at a material is required and the light microscope no longer provides adequate resolution. In the SEM an electron beam is focused into a fine probe and subsequently raster scanned over a small rectangular area. As the beam interacts with the sample it creates various signals (secondary electrons, internal currents, photon emission, etc.), all of which can be appropriately detected. These signals are highly localized to the area directly under the beam. By using these signals to modulate the brightness of a cathode ray tube, which is raster scanned in synchronism with the electron beam, an image is formed on the screen. This image is highly magnified and usually has the U1~~k" of a traditional microscopic image but with a much greater depth of field. With ancillary detectors, the instrument is capable of elemental analysis. Main use High magnification imaging and composition (elemental) mapping No, some electron beam damage 10~-300,000~; 5000~-100,000~ is the typical operating range 500 eV-50 keV; typically, 20-30 keV conducting film; must be vacuum compatible Less than O.lmm, up to 10 cm or more 1-50 nm in secondary electron mode Varies from a few nm to a few pm, depending upon the accelerating voltage and the mode of analysis Destructive Magnification range Beam energy range Sample requirements Minimal, occasionally must be coated with a Sample size Lateral resolution Depth sampled Bonding information No Depth profiling Only indirect capabilities Instrument cost $100,000-$300,000 is typical Size Electronics console 3 ft. x 5 fi.; electron beam column 3 ft. x 3 ft. 8 INTRODUCTION AND SUMMARIES Chapter 1
Scanning Tunneling Microscopy and Scanning Force Microscopy (STM and SFM) 1.2.3 In Scanning Tunneling Microscopy(STM)or Scanning Force Microscopy(SFM), a solid in air.liquid or d within a surface In'STM. quantu mecha ing current floy between atoms on the surface and thos e on the tip.In SFM,also kno wn as Atomi Force Microscopy (AFM),interatomic forces between the atoms on the surface and those on the tip cause the deflection of a microfabricated cantilever.Because the magnitude of the tunneling current or cantilever deflection depends strongly upon separation bet een the surface and ti atoms.the ey can be sed to r nic ion in all thre e dimensions. The tunne ng cu n of loc ele ctronic structure so that atomic-scale spectroscopy is possible.Both STM and SFM are unsurpassed as high-resolution, three-dimensional profilometers. rehy(SFM and STM):loca eon Parameters measured Surface to Destructive No Vertical resolution STM,0.01 A:SFM,0.1A Lateral resolution STM,atomic;SFM,atomic to I nm Quantification Yes:three-dimensional Accuracy Better than 10%in distance Imaging/mapping Yes Field of view From atoms to>250 um Sample requirements STM-solid conductors and semiconductors,conductive coating equired for insulators;SFM-solid conductors semiconductors and insulators Main uses Real-space three-dimensional imagi in air. vacuu tion;high-resolution profilometry;imaging of nonconductors(SFM). Instrument cost $65,000 (ambient)to $200,000 (ultrahigh vacuum) Size Table-top (ambient),2.27-12 inch bolt-on flange (ultrahigh vacuum)
Scanning Tunneling Microscopy and Scanning Force Microscopy (STM and SFM) 1.2.3 In Scanning Tunneling Microscopy (STM) or Scanning Force Microscopy (SFM), a solid specimen in air, liquid or vacuum is scanned by a sharp tip located within a few A of the surface. In STM, a quantum-mechanical tunneling current flows between atoms on the surface and those on the tip. In SFM, also known as Atomic Force Microscopy (AFM), interatomic forces between the atoms on the surface and those on the tip cause the deflection of a microfabricated cantilever. Because the magnitude of the tunneling current or cantilever deflection depends strongly upon the separation between the surface and tip atoms, they can be used to map out surface topography with atomic resolution in all three dimensions. The tunneling current in STM is also a function of local electronic structure so that atomic-scale spectroscopy is possible. Both STM and SFM are unsurpassed as high-resolution, three-dimensional profilometers. Parameters measured Surface topography (SFM and STM); local electronic Destructive No Vertical resolution Lateral resolution Quantification Yes; three-dimensional Accuracy Imaging/mapping Yes Field of view From atoms to > 250 pm Sample requirements STM-solid conductors and semiconductors, conductive coating required for insulators; SFM-solid conductors, semiconductors and insulators structure (STM) STM, 0.01 8; SFM, 0.1 A STM, atomic; SFM, atomic to 1 nm Better than 10% in distance Main uses Real-space three-dimensional imaging in air, vacuum, or solution with unsurpassed resolution; high-resolution profilometry; imaging of nonconductors (SFM). Instrument cost Size $65,000 (ambient) to $200,000 (ultrahigh vacuum) Table-top (ambient), 2.27-12 inch bolt-on flange (ultrahigh vacuum) 9