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Journal articles on the topic 'Electron beam microanalysis'

Author: Grafiati

Published: 4 June 2021

Last updated: 19 February 2022

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1

Howitt, D. G., and D. L. Medlin. "Beam Induced Composition Modifications During Electron Beam Microanalysis." Microscopy and Microanalysis 4, S2 (July 1998): 228–29. http://dx.doi.org/10.1017/s1431927600021267.

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The most common cause of composition modification to a specimen during electron probe microanalysis is the field induced migration of light elements. This is an indirect effect which occurs in response to the long range electric fields that form when dielectric specimens suffer charge imbalance. The result is that the ions are redistributed within the sample according to their respective mobilities and the affect is enhanced rather than eliminated when the sample is coated. The ions typically move radially outward in thin samples because of the excess production of secondary electrons from the specimen surfaces, Cazaux(1986)and downwards in conventional SEM samples when the field is due primarily to the deposition of electrons within the bulk of the specimenField induced migration is responsible for most of the elemental signal variations observed during the microanalysis of silicate glasses containing sodium or potassium ions.

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2

Stevens Kalceff, Marion A. "Irradiation Induced Effects in the Environmental Scanning Electron Microscope." Microscopy and Microanalysis 5, S2 (August 1999): 276–77. http://dx.doi.org/10.1017/s1431927600014707.

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When a poorly conducting specimen is irradiated with an electron beam in a variable pressure electron microscope, the excess charge on the surface of the specimen can be neutralized by incident gas ions to prevent deflection and retarding of the electron beam. A small fraction (<10∼6) of the incident electrons are trapped at irradiation induced or pre-existing defects within the irradiated micro-volume of specimen. The trapped charge induces an electric field, which may result in the electro-migration and micro-segregation of charged mobile defect species within the irradiated volume of specimen. These charge induced effects are dependent on the density of trapping centers and their capture cross sections. In particular, evidence of these micro-diffusion processes can be directly observed in electron beam irradiated ultra pure silicon dioxide (SiO2) polymorphs using Cathodoluminescence (CL) microanalysis (spectroscopy and imaging). CL microanalysis enables both pre-existing and irradiation induced defects in wide band gap materials (i.e. semiconductors and insulators) to be monitored and characterized with high sensitivity and spatial resolution. Depth resolution is achieved by varying the electron beam energy.

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3

Meisenkothen, Frederick, Robert Wheeler, Michael D. Uchic, Robert D. Kerns, and Frank J. Scheltens. "Electron Channeling: A Problem for X-Ray Microanalysis in Materials Science." Microscopy and Microanalysis 15, no. 2 (March 16, 2009): 83–92. http://dx.doi.org/10.1017/s1431927609090242.

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AbstractElectron channeling effects can create measurable signal intensity variations in all product signals that result from the scattering of the electron beam within a crystalline specimen. Of particular interest to the X-ray microanalyst are any variations that occur within the characteristic X-ray signal that are not directly related to a specimen composition variation. Many studies have documented the effect of crystallographic orientation on the local X-ray yield; however, the vast majority of these studies were carried out on thin foil specimens examined in transmission. Only a few studies have addressed these effects in bulk specimen materials, and these analyses were generally carried out at common scanning electron microscope microanalysis overvoltages (>1.5). At these overvoltage levels, the anomalous transmission effect is weak. As a result, the effect of electron channeling on the characteristic X-ray signal intensity has traditionally been overlooked in the field of quantitative electron probe microanalysis. The present work will demonstrate that electron channeling can produce X-ray variations of up to 26%, between intensity maxima and minima, in low overvoltage X-ray microanalyses of bulk specimens. Intensity variations of this magnitude will significantly impact the accuracy of qualitative and quantitative X-ray microanalyses at low overvoltage on engineering structural materials.

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4

Santala, M., B. Reed, T. LaGrange, G. Campbell, and N. Browning. "Dynamic Convergent Beam Electron Diffraction." Microscopy and Microanalysis 17, S2 (July 2011): 508–9. http://dx.doi.org/10.1017/s1431927611003412.

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5

Ottensmeyer, F. P., and X. G. Jiang. "High-resolution electron spectrometers for molecular microanalysis." Proceedings, annual meeting, Electron Microscopy Society of America 46 (1988): 664–65. http://dx.doi.org/10.1017/s0424820100105382.

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The last decade has brought major advances in electron beam induced microanalytical capabilities, particularly with the utilization of energy loss electrons. These developments have been predicated primarily by the design and by the more ready commercial availabilty of better magnetic spectrometers, both for scanning transmission and fixed-beam transmission electron microscopy.Theoretical and experimental investigation of spatial resolution or localization possible for microanalysis and elemental mapping has indicated a potential of about 0.5 nm at an energy loss close to 100 eV, improving slowly with increasing energy loss. At lower energy loss the spatial resolution worsens due to an expected increase in impact parameter, but is still anticipated to be of the order of 1 nm at a 10 eV loss.Coupled with high spatial resolution is an experimentally observed very high sensitivity of detection and identification of a very small number of atoms at high concentration.

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6

Stevens Kalceff, M. A., M. R. Phillips, and A. R. Moon. "Cathodoluminescence Investigation of Electron Irradiation Damage in Insulators." Microscopy and Microanalysis 3, S2 (August 1997): 749–50. http://dx.doi.org/10.1017/s1431927600010631.

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Cathodoluminescence (CL) is the luminescent emission from a material which has been irradiated with electrons. Cathodoluminescence microanalysis (spectroscopy and microscopy) in an electron microscope complements the average defect structure information available from complementary techniques (e.g. Photoluminescence, Electron Spin Resonance spectroscopy). CL microanalysis enables both pre-existing and irradiation induced local variations in the bulk and surface defect structure to be characterized with high spatial (lateral and depth) resolution and sensitivity. This is possible as electron beam parameters such as the beam energy, may be varied to finely control the penetration depth of the incident electrons and hence the local volume of specimen probed.Irradiation with charged and neutral energetic radiation produces defects in radiation sensitive materials. The energetic electron beam in an electron microscope may also induce defects in the specimen. Cazaux has characterized the electric field produced by electron irradiation of a insulator with a conductive surface coating

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7

Carlton, Robert A., Charles E. Lyman, James E. Roberts, and Raynald Gauvin. "Evaluation of Corrections for X-Ray Microanalysis in the ESEM." Microscopy and Microanalysis 7, S2 (August 2001): 698–99. http://dx.doi.org/10.1017/s1431927600029561.

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A number of methods have been proposed to correct for the electron beam scattering effects on xray microanalysis in the environmental scanning electron microscope (ESEM). This paper presents an evaluation of two of these methods. The Doehne method is based on the observation that x-ray counts due to the unscattered electron beam increase with decreasing chamber pressure whereas the inverse is true for x-ray counts due to scattered electrons. The x-ray count intercept, at zero pressure, of the regression lines relating x-ray counts to chamber vapor pressure is an estimate of the high-vacuum intensity. The Gauvin method is based on the relationship between x-ray counts and the fraction of the electron beam that is unscattered, fp.The fraction of the unscattered beam is calculated using an equation derived from scattering theory and uses the accelerating voltage, the gas path length, and the chamber vapor pressure.

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8

Kasama, Takeshi, Rafal E. Dunin-Borkowski, Simon B. Newcomb, and Martha R. McCartney. "Electron Beam Induced Charging of Focused Ion Beam Milled Semiconductor Transistors Examined Using Electron Holography." Microscopy and Microanalysis 10, S02 (August 2004): 988–89. http://dx.doi.org/10.1017/s1431927604883132.

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9

Garratt-Reed, Anthony J. "Microanalysis of boundaries by AEM at different voltages." Proceedings, annual meeting, Electron Microscopy Society of America 51 (August 1, 1993): 600–601. http://dx.doi.org/10.1017/s0424820100148836.

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It is well known that theory predicts a number of benefits for high-resolution analytical electron microscopy (AEM) in raising the electron energy. These benefits arise from three principal effects, namely, an anticipated linear decrease in the beam broadening in the foil with increasing energy, and an increase in the electron gun brightness with increasing energy, and an increase in the X-ray peak-tobackground ratio as the electron energy is raised. In addition, the decrease in the electron wavelength with increasing energy can also lead to improvement in the image resolution, although generally not in the microanalytical resolution. To set off against these benefits is the disadvantage that the ionization cross-section decreases with increasing beam voltage. However, although for the case of nonrelativistic electrons this can be a significant effect, in most cases, for relativistic electrons (those used for intermediate-voltage AEM, for example) this decrease is not severe. For example, fig. 1 plots the ionization cross-section for iron for electrons in the range 20-500kV, according to the relativistic equation of Chapman et. al. A further area of interest is the effect of radiation damage in the sample, which may increase or decrease at higher voltages.

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10

Gauvin, Raynald. "X-Ray Microanalysis of Materials in the ESEM or VP-SEM." Microscopy and Microanalysis 7, S2 (August 2001): 778–79. http://dx.doi.org/10.1017/s1431927600029962.

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When performing X-Ray microanalysis in the ESEM (Environmental Scanning Electron Microscope) or in the VP-SEM (Variable Pressure Scanning Electron Microscope), the operating conditions of the microscope must be optimized. This is to reduce the beam broadening of the incident electrons when they scatter with the gas molecules before entering into the specimen. As a result of this scattering, the incident beam is composed of two parts. The first part of the beam is the unscattered beam and the second part is the scattered beam, named the skirt. in high pressure and long working distances conditions, the diameter of the skirt may extend to several millimeters. in order to show the effect of the skirt on X-Ray generation, a copper strip was placed .5 mm away of the electron beam on a flat Al specimen. The peak to background ratio of the copper line was measured at different pressure (from 25 to 200 Pa) for Air as gas.

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11

Liao, Y., and L. D. Marks. "EDS Assisted by Precessing Electron Beam." Microscopy and Microanalysis 19, S2 (August 2013): 1274–75. http://dx.doi.org/10.1017/s1431927613008362.

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12

LeBeau, J., S. Findlay, L. Allen, and S. Stemmer. "Position Averaged Convergent Beam Electron Diffraction." Microscopy and Microanalysis 15, S2 (July 2009): 494–95. http://dx.doi.org/10.1017/s1431927609096743.

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13

Kruit, P. "Novel Methods of Microanalysis Employing Secondary- and Auger-Electron Spectroscopy in Stem." Proceedings, annual meeting, Electron Microscopy Society of America 48, no. 1 (August 12, 1990): 214–15. http://dx.doi.org/10.1017/s0424820100179828.

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Introduction: Electron spectroscopy is a well established technique in physics and material science and merely adding the spatial resolution of a STEM would already open a new field of applications. However, by using the specific advantages of electron microscope optics and the expertise in thin specimen preparation of microscopists, electron spectroscopy in the STEM can yield information that cannot be obtained in any other way.Instrumentation: The feasibility of extracting a large portion of the Auger and secondary electrons from the magnetic field of an immersion condenser objective lens has now been demonstrated. The scheme involves a careful shaping of the magnetic field through which the electrons are guided to a deflector which separates the secondary beam from the primary beam. The parallelizing action of this field forces the electrons into a beam of small opening angle which can be accepted by traditional optics including an electrostatic energy analyser. Results reported in this paper are from a prototype instrument; energy analysers mounted on fully ultra high vacuum microscopes are now also in operation or will become operational very soon. To detect the secondary or Auger electron together with the primary electron which was responsible for its emission requires only small additions to the instrumentation. Single electron sensitivity in both the secondary electron detector and the EELS detector are of course necessary, but this can be done with standard detectors with a timing resolution of better than 5 ns. Commercial electronic equipment can then sort the coincident events.

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14

Toth, M., R. Knowles, G. Hartigan, and C. Lobo. "Electron Flux Controlled Switching Between Electron Beam Induced Etching and Deposition." Microscopy and Microanalysis 12, S02 (July 31, 2006): 168–69. http://dx.doi.org/10.1017/s1431927606069753.

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15

Mittal, A., and K. A. Mkhoyan. "Electron Beam Channeling in Single Atomic Column." Microscopy and Microanalysis 19, S2 (August 2013): 604–5. http://dx.doi.org/10.1017/s1431927613005011.

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16

Fitting, H.-J., and M. Touzin. "Fast Electron Beam Switching in Dielectric Samples." Microscopy and Microanalysis 16, S2 (July 2010): 264–65. http://dx.doi.org/10.1017/s1431927610053675.

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17

Jiang, N. "Electron-Beam Fabrication of Nanostructures in Glasses." Microscopy and Microanalysis 16, S2 (July 2010): 1660–61. http://dx.doi.org/10.1017/s1431927610056540.

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18

Lyman, Charles E., Robert A. Carlton, and James E. Roberts. "Quantitative X-Ray Microanalysis of Uncoated Ceramics." Microscopy and Microanalysis 7, S2 (August 2001): 436–37. http://dx.doi.org/10.1017/s1431927600028257.

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Uncoated ceramics are difficult to analyze because specimen charging can reduce the energy of the electron beam at the specimen. This effect may decrease the measured k-ratio to a fraction of its expected value. Thin carbon coatings are the usual solution to this problem. However, the coating procedure takes time, and the same coating thickness also must be applied to the standard. in the environmental SEM (ESEM). surface charge can be mitigated at the higher accelerating voltages normally used for x-ray microanalysis. in the ESEM, electrons are accelerated toward an electrically biased electron detector producing a cascade of electrons and ions from the imaging gas (water vapor) as part of the secondary electron imaging process. Positive ions drift toward the specimen and neutralize negative surface charge; however, the degree of neutralization is a function of a number of operating variables.

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19

Williams, David B., and S. Michael Zemyan. "Microanalysis At Intermediate Voltages." Proceedings, annual meeting, Electron Microscopy Society of America 48, no. 1 (August 12, 1990): 480–81. http://dx.doi.org/10.1017/s0424820100181154.

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Microanalysis using x-ray emission spectrometry (XES) or electron energy-loss spectrometry (EELS) at intermediate voltages should offer advantages over 100kV instruments. Brightness increases linearly with kV (for thermionic sources), but the inelastic scattering cross section decreases. Potential improvements in detectability limit and spatial resolution in both XES and EELS have been major factors spurring the development of intermediate voltage AEMs.The x-ray peak to background ratio increases with kV (Figure 1), and improvements in detectability limits have been reported at 300kV. The variation of detectability with spatial resolution is discussed elsewhere in these proceedings. Beam spreading should decrease linearly with kV, but experimentally the spatial resolution (Figure 2a,2b) does not show the expected improvement. This may be due to increased beam broadening from fast secondary electrons. The smallest probe size consistent with generating sufficient signal (i.e. an FEG) is better than increased kV for improved spatial resolution3. Increased kV has seen the return of the ‘hole count’ problem in XES. Higher voltage electrons generate harder x-rays at the C aperture, and current aperture design cannot sufficiently restrict the xray flux. The flux at 300kV can contribute up to 10% of the characteristic x-ray signal, which severely compromises the microanalysis quality. An FEG with reduced source size may help. At intermediate voltages, intrinsic Ge (IG) detectors can be used for analysis of Kα, lines from high atomic number elements. K line analysis gives improved accuracy compared with L and M line analysis for which Cliff- Lorimer k factors, (both experimental and theoretical) are extremely variable, possibly due to fast secondaries also. IG detectors can detect Au K lines, resolve Kα1Kα2 lines, (see Figure 3) offer improved energy resolution (~120eV) over Si(Li) detectors, and may be more stable under electron irradiation. Continued improvement in IG detectors may result in their displacing Si(Li) detectors from most AEMs.

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20

Krishnan, Kannan M. "Crystallographic Effect in X-Ray Microanalysis." Proceedings, annual meeting, Electron Microscopy Society of America 48, no. 2 (August 12, 1990): 466–67. http://dx.doi.org/10.1017/s0424820100135939.

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The interaction of a fast electron, accelerated through kilovolt potentials in an electron microscope, with a thin foil sample will produce a variety of signals that can be monitored with appropriate detectors to provide information about the crystallography, chemistry and electronic structure of trie sample. In particular, the characteristic x-ray emissions are well understood and form the basis of a simple microanalytical technique by relating the measured x-ray intensities (IA,B) to the elemental weight fractions (CA,B) using the ratio method originally proposed by Cliff and Lorimer , i.e. CA / CB = KAB * IA / IB. This formulation makes the assumption that all the possible atomic sites for the two elements (A and B) in the sample are probed with the same probability by the incident electron beam.The above assumption is not valid for crystalline samples illuminated with a parallel beam of electrons under strong dynamical diffraction conditions.

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21

Barkshire, I. R., P. Karduck, W. Rehbach, and S. Richter. "High Spatial Resolution Low Energy Electron Beam X-ray Microanalysis." Microscopy and Microanalysis 5, S2 (August 1999): 310–11. http://dx.doi.org/10.1017/s1431927600014872.

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Conventionally, x-ray microanalysis on scanning electron microscopes (SEM) with energy dispersive spectrometers (EDS) has been performed with relatively high primary energies (>10 kv). for most samples this results in reasonably good separation of the generated x-ray line series from different elements enabling unambiguous identification and therefore accurate qualitative analysis. Under these circumstances it is widely accepted that quantitative analysis of polished bulk samples is possible on a routine basis with relative errors around 1-5% and detection limits of the order of 0.1%.However, in order to address the analysis requirements of new advanced materials with sub-micron features, there is growing interest in performing x-ray microanalysis at low beam energies(<5kv). this is now a more realistic goal due to the routine availability of field emission sem's which can operate with much improved beam sizes at low beam energies with sufficient beam current to perform practical microanalysis, in conjunction with the improved low energy performance of current, commercially available EDS systems.

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22

Kubo, Y. "Focussed ion beam thin sample microanalysis using a field emission gun electron probe microanalyser." IOP Conference Series: Materials Science and Engineering 304 (January 2018): 012007. http://dx.doi.org/10.1088/1757-899x/304/1/012007.

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23

Su, D., F. Wang, C. Ma, and N. Jiang. "Electron-Beam-Induced Structure transition in spinel Li4Ti5O12." Microscopy and Microanalysis 18, S2 (July 2012): 1488–89. http://dx.doi.org/10.1017/s1431927612009294.

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24

Grogan, J. M., F. M. Ross, and H. H. Bau. "Beam-Sample Interactions During Liquid Cell Electron Microscopy." Microscopy and Microanalysis 19, S2 (August 2013): 408–9. http://dx.doi.org/10.1017/s1431927613004030.

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25

Barkman, J. E., P. Carpenter, J. C. Zhao, and J. J. Donovan. "Electron Microprobe Quantitative Mapping vs. Defocused Beam Analysis." Microscopy and Microanalysis 19, S2 (August 2013): 848–49. http://dx.doi.org/10.1017/s1431927613006235.

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26

Kizilyaprak, C., C. Loussert, J. Daraspe, and B. M. Humbel. "Focussed Ion Beam Scanning Electron Microscopy in Biology." Microscopy and Microanalysis 19, S2 (August 2013): 874–75. http://dx.doi.org/10.1017/s1431927613006363.

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27

Egerton, RF. "Mechanisms of Radiation Damage and Electron-Beam Fabrication." Microscopy and Microanalysis 16, S2 (July 2010): 1658–59. http://dx.doi.org/10.1017/s1431927610055182.

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28

Reyes-Coronado, A., J. Aizpurua, PM Echenique, RG Barrera, and PE Batson. "Plasmon Driven Nanoparticle Movement in the Electron Beam." Microscopy and Microanalysis 16, S2 (July 2010): 1766–67. http://dx.doi.org/10.1017/s1431927610061775.

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29

Mulders, JJ L. "New Electron and Ion Beam Chemistry for Nanotechnology." Microscopy and Microanalysis 12, S02 (July 31, 2006): 1288–89. http://dx.doi.org/10.1017/s1431927606068413.

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30

Fowlkes, JD, DA Smith, and PD Rack. "Electron Beam Induced Processing: Experimentation, Simulation, and Applications." Microscopy and Microanalysis 14, S2 (August 2008): 1196–97. http://dx.doi.org/10.1017/s1431927608083633.

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31

Kruit, P., W. van Dorp, K. Hagen, and PA Crozier. "Synthesis of Nanostructures using Electron Beam Induced Deposition." Microscopy and Microanalysis 14, S2 (August 2008): 242–43. http://dx.doi.org/10.1017/s1431927608084511.

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32

Li, J., and I. Anderson. "Rocking-Beam Variable Coherence Electron Microscopy: An Alternative Approach to Fluctuation Electron Microscopy." Microscopy and Microanalysis 12, S02 (July 31, 2006): 672–73. http://dx.doi.org/10.1017/s1431927606067316.

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33

Tousimis, A. J. "The Basic Physical Principles of Ion, Electron, and X-Ray Detectors and Their Application to Microanalysis." Proceedings, annual meeting, Electron Microscopy Society of America 43 (August 1985): 154–57. http://dx.doi.org/10.1017/s0424820100117777.

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An integral and of prime importance of any microtopography and microanalysis instrument system is its electron, x-ray and ion detector(s). The resolution and sensitivity of the electron microscope (TEM, SEM, STEM) and microanalyzers (SIMS and electron probe x-ray microanalyzers) are closely related to those of the sensing and recording devices incorporated with them.Table I lists characteristic sensitivities, minimum surface area and depth analyzed by various methods. Smaller ion, electron and x-ray beam diameters than those listed, are possible with currently available electromagnetic or electrostatic columns. Therefore, improvements in sensitivity and spatial/depth resolution of microanalysis will follow that of the detectors. In most of these methods, the sample surface is subjected to a stationary, line or raster scanning photon, electron or ion beam. The resultant radiation: photons (low energy) or high energy (x-rays), electrons and ions are detected and analyzed.

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34

Matthews, Mike B., Stuart L. Kearns, and Ben Buse. "Electron Beam-Induced Carbon Erosion and the Impact on Electron Probe Microanalysis." Microscopy and Microanalysis 24, no. 6 (November 16, 2018): 612–22. http://dx.doi.org/10.1017/s1431927618015398.

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AbstractElectron beam-induced carbon contamination is a balance between simultaneous deposition and erosion processes. Net erosion rates for a 25 nA 3 kV beam can reduce a 5 nm C coating by 20% in 60 s. Measurements were made on C-coated Bi substrates, with coating thicknesses of 5–20 nm, over a range of analysis conditions. Erosion showed a step-like increase with increasing electron flux density. Both the erosion rate and its rate of change increase with decreasing accelerating voltage. As the flux density decreases the rate of change increases more rapidly with decreasing voltage. Time-dependent intensity (TDI) measurements can be used to correct for errors, in both coating and substrate quantifications, resulting from carbon erosion. Uncorrected analyses showed increasing errors in coating thickness with decreasing accelerating voltage. Although the erosion rate was found to be independent of coating thickness this produces an increasing absolute error with decreasing starting thickness, ranging from 1.5% for a 20 nm C coating on Bi at 15 kV to 14% for a 5 nm coating at 3 kV. Errors in Bi Mα measurement are <1% at 5 kV or above but increase rapidly below this, both with decreasing voltage and increasing coating thickness to 20% for a 20 nm coated sample at 3 kV.

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35

McKeown, JT, and JCH Spence. "Nanocrystal Structure Determination by Kinematic Convergent-Beam Electron Diffraction." Microscopy and Microanalysis 15, S2 (July 2009): 758–59. http://dx.doi.org/10.1017/s1431927609094495.

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36

Liu, Z. Q., K. Mitsuishi, and K. Furuya. "Nanofabrication of Tungsten Structure by Electron-Beam-Induced Deposition in Scanning Transmission Electron Microscope." Microscopy and Microanalysis 10, S02 (August 2004): 566–67. http://dx.doi.org/10.1017/s1431927604883831.

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37

Wooten, JR, and DP Dennies. "Microstructural Evaluation of Electron Beam Melted Ti-6Al-4V." Microscopy and Microanalysis 14, S2 (August 2008): 616–17. http://dx.doi.org/10.1017/s1431927608082792.

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38

McMorran, B., and A. Cronin. "Measurement of Electron Beam Coherence Using a Lau Interferometer." Microscopy and Microanalysis 14, S2 (August 2008): 828–29. http://dx.doi.org/10.1017/s1431927608087473.

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39

Eder, F., J. C. Meyer, S. Kurasch, U. Kaiser, V. Skakalova, J. Kotakoski, A. V. Krashenninikov, and A. Chuvilin. "Quantitative Analysis of Electron Beam-Induced Destruction of Graphene Membranes under an Electron Microscope." Microscopy and Microanalysis 18, S2 (July 2012): 1500–1501. http://dx.doi.org/10.1017/s143192761200935x.

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Liu, Z.-Q., K. Mitsuishi, and K. Furuya. "Influence of Beam Energy and Probe Size on the Process of Electron-Beam-Induced Deposition." Microscopy and Microanalysis 12, S02 (July 31, 2006): 646–47. http://dx.doi.org/10.1017/s143192760606510x.

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Blackson, J. H., D. W. Susnitzky, and D. R. Beaman. "Extending the limits of molecular microanalysis." Proceedings, annual meeting, Electron Microscopy Society of America 52 (1994): 946–47. http://dx.doi.org/10.1017/s0424820100172462.

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Modern polymer blends are frequently composed of domains and interfacial phases having submicron dimensions. Previously, die characterization of specific unknown submicron polymer phases has been limited to selective staining methods that help to classify the phase but rarely lead to chemical identification. The present procedure uses parallel detection electron energy loss spectroscopy (PEELS) to perform submicron molecular microanalysis on beam sensitive materials. Polymer domains are first differentiated by their elemental composition and then by their characteristic carbon core loss edge structure. These spectra are compared to spectra recorded from polymers of known composition.A polymer film composed of alternating 0.5 μm layers of polycarbonate (PC) and polymethylmethacrylate (PMMA) was used as a test specimen (Fig. 1). Ultra-thin sections (<50 nm) were prepared by microtomy, collected on unsupported 600 mesh copper grids and examined at −160°C usinga VG HB601UX dedicated STEM fitted with a Gatan 666 UHV PEELS. The combination of beam blanking, simplecontrol of electron dose, UHV, low energy spread FEG, stage stability and the ability to produce a high contrast image at a very low electron dose makes this instrument ideally suited for this experiment.

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42

Joy, David C. "Fundamental Constants for Quantitative X-ray Microanalysis." Microscopy and Microanalysis 7, no. 2 (March 2001): 159–67. http://dx.doi.org/10.1007/s100050010070.

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Abstract Quantitative X-ray microanalysis requires the use of many fundamental constants related to the interaction of the electron beam with the sample. The current state of our knowledge of such constants in the particular areas of electron stopping power, X-ray ionization cross-sections, X-ray fluorescence yield, and the electron backscattering yield, is examined. It is found that, in every case, the quality and quantity of data available is poor, and that there are major gaps remaining to be filled.

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Wight, S., D. Meier, M. Postek, A. Vladar, J. Small, and D. Newbury. "He Ion Induced Secondary Electron and Backscattered Electron Images Compared Side-by-side With Electron Beam Induced Secondary Electron, Backscattered, and Transmission Electron Images." Microscopy and Microanalysis 14, S2 (August 2008): 1186–87. http://dx.doi.org/10.1017/s1431927608088727.

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44

Newbury, D. E., and R. B. Marinenko. "Accuracy barriers of quantitative electron beam x-ray microanalysis - Foreword." Journal of Research of the National Institute of Standards and Technology 107, no. 6 (November 2002): v. http://dx.doi.org/10.6028/jres.107.001.

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Nockolds, C. E. "Characteristic and Continuum Fluorescence in Electron Beam X-ray Microanalysis." Microscopy and Microanalysis 5, S2 (August 1999): 562–63. http://dx.doi.org/10.1017/s1431927600016135.

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Of the different aspects of electron probe microanalysis(EPMA)which were studied by Castaing during his doctorate the work on characteristic x-ray fluorescence was the most definitive. In his thesis, which was completed in 1951, Castaing established the physical and mathematical framework for a correction procedure for fluorescence which is essentially still used in EPMA today. Much of the effort since then has been in refining and improving the accuracy of the correction and extending the scope of the correction to a wider range of specimen types. The Castaing formula was developed for the case of a K x-ray from element A being excited by a K xray from element B (K-K fluorescence) and in 1965 Reed extended the range of the correction by including the K-L, L-L and L-K interactions. In the same paper Reed also introduced the expression from Green and Cosslett for the calculation of K intensities, which was believed to be more accurate than the expression used by Castaing. The original formula included a somewhat unrealistic exponential term to allow for the depth of the production of the primary x-rays and a number of workers have tried replacing this term with a more accurate expression, however, in general this has led to only small changes in the final correction. Reed also simplified the formula in order to make the calculation easier in the days before fast computers; in particular he replaced the jump ratio variable by two constants, one for the K-shell and one for the L-shell. Much later Heinrich showed that this simplification was no longer necessary and that the jump ratio could in fact be calculated directly.

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Newbury, Dale E., and Nicholas W. M. Ritchie. "Quantitative Electron-Excited X-ray Microanalysis at Low Beam Energy." Microscopy and Microanalysis 21, S3 (August 2015): 1875–76. http://dx.doi.org/10.1017/s1431927615010156.

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Barkshire, Ian, Peter Karduck, Werner P. Rehbach, and Silvia Richter. "High-Spatial-Resolution Low-Energy Electron Beam X-Ray Microanalysis." Microchimica Acta 132, no. 2-4 (April 2000): 113–28. http://dx.doi.org/10.1007/s006040050052.

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Egerton, R. F., and P. A. Crozier. "Erosion of TEM Specimens in an Intense Electron Beam." Microscopy and Microanalysis 10, S03 (August 2004): 54–55. http://dx.doi.org/10.1017/s143192760455568x.

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Extended abstract of a paper presented at the Pre-Meeting Congress: Materials Research in an Aberration-Free Environment, at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, July 31 and August 1, 2004.

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Boyes, E. D. "On Low Voltage Scanning Electron Microscopy and Chemical Microanalysis." Microscopy and Microanalysis 6, no. 4 (July 2000): 307–16. http://dx.doi.org/10.1017/s1431927602000545.

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AbstractThe current status and general applicability of scanning electron microscopy (SEM) at low voltages is reviewed for both imaging (low voltage scanning electron microscopy, LVSEM) and chemical microanalysis (low voltage energy-dispersive X-ray spectrometry, LVEDX). With improved instrument performance low beam energies continue to have the expected advantages for the secondary electron imaging of low atomic number (Z) and electrically non-conducting samples. They also provide general improvements in the veracity of surface topographic analysis with conducting samples of all Z and at both low and high magnifications. In new experiments the backscattered electron (BSE) signal retains monotonic Z dependence to low voltages (<1 kV). This is contrary to long standing results in the prior literature and opens up fast chemical mapping with low dose and very high (nm-scale) spatial resolution. Similarly, energy-dispersive X-ray chemical microanalysis of bulk samples is extended to submicron, and in some cases to <0.1 μm, spatial resolution in three dimensions at voltages <5 kV. In favorable cases, such as the analysis of carbon overlayers at 1.5 kV, the thickness sensitivity for surface layers is extended to <2 nm, but the integrity of the sample surface is then of concern. At low beam energies (E0) the penetration range into the sample, and hence the X-ray escape path length out of it, is systematically restricted (R = F(E05/3)), with advantages for the accuracy or elimination of complex analysis-by-analysis matrix corrections for absorption (A) and fluorescence (F). The Z terms become more sensitive to E0 but they require only one-time calibrations for each element. The new approach is to make the physics of the beam–specimen interactions the primary factor and to design enabling instrumentation accordingly.

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Boyes, E. D. "On Low Voltage Scanning Electron Microscopy and Chemical Microanalysis." Microscopy and Microanalysis 6, no. 4 (July 2000): 307–16. http://dx.doi.org/10.1007/s100050010035.

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Abstract:

Abstract The current status and general applicability of scanning electron microscopy (SEM) at low voltages is reviewed for both imaging (low voltage scanning electron microscopy, LVSEM) and chemical microanalysis (low voltage energy-dispersive X-ray spectrometry, LVEDX). With improved instrument performance low beam energies continue to have the expected advantages for the secondary electron imaging of low atomic number (Z) and electrically non-conducting samples. They also provide general improvements in the veracity of surface topographic analysis with conducting samples of all Z and at both low and high magnifications. In new experiments the backscattered electron (BSE) signal retains monotonic Z dependence to low voltages (<1 kV). This is contrary to long standing results in the prior literature and opens up fast chemical mapping with low dose and very high (nm-scale) spatial resolution. Similarly, energy-dispersive X-ray chemical microanalysis of bulk samples is extended to submicron, and in some cases to <0.1 μm, spatial resolution in three dimensions at voltages <5 kV. In favorable cases, such as the analysis of carbon overlayers at 1.5 kV, the thickness sensitivity for surface layers is extended to <2 nm, but the integrity of the sample surface is then of concern. At low beam energies (E0) the penetration range into the sample, and hence the X-ray escape path length out of it, is systematically restricted (R = F(E05/3)), with advantages for the accuracy or elimination of complex analysis-by-analysis matrix corrections for absorption (A) and fluorescence (F). The Z terms become more sensitive to E0 but they require only one-time calibrations for each element. The new approach is to make the physics of the beam–specimen interactions the primary factor and to design enabling instrumentation accordingly.

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