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Materials Characterization

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Materials Chemistry
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Abstract

Thus far, we have focused on the relationship between the structure of a material and its properties/applications. However, we have not yet focused on how one is able to determine the structure and composition of materials. That is, when a material is fabricated in the lab, how are we able to assess whether our method was successful? Depending on the nature of the material being investigated, a suite of techniques may be utilized to assess its structure and properties. Whereas some techniques are qualitative, such as providing an image of a surface, others yield quantitative information such as the relative concentrations of atoms that comprise the material. Recent technological advances have allowed materials scientists to accomplish something that was once thought to be impossible: to obtain actual two-dimensional/threedimensional images of atomic positions in a solid, in real time. It should be noted that the sensitivity of quantitiative techniques also continues to be improved, with techniques now being able to easily measure parts per trillion (ppt) concentrations of impurities in a bulk sample.

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References and Notes

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  76. Many references exist for MIES studies of surfaces, most often carried out in tandem with UPS (to gain information for both the surface and immediate subsurface of the sample). For example, see: (a) Johnson, M. A.; Stefanovich, E. V.; Truong, T. N.; Gunster, J.; Goodman, D. W. J. Phys. Chem. B 1999, 103, 3391. (b) Kim, Y. D.; Wei, T.; Stulz, J.; Goodman, D. W. Langmuir 2003, 19, 1140 (very nice work that describes the shortfall of UPS alone, and the utility of a tandem UPS/MIES approach).

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  77. Though conventional RBS is carried out with He+ ions (which will backscatter from any atom with a greater Z ), heavier ions such as C, O, Si, or Cl may be used in order to prevent background backscattering interactions with the matrix. For example, use of incident O ions to eliminate backscattering from lattice O atoms for the RBS analysis of ceramic oxides.

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  78. Simulations for ion scattering techniques such as RBS are typically compared with actual spec- tra in order to characterize the surface features. There are many such algorithms; for example: (a) Kido, Y.; Koshikawa, T. J. Appl. Phys. 1990, 67, 187. (b) Doolittle, L. R. Nucl. Instrum. Methods 1986, B 15, 227 (RUMP program). (c) http://www.ee.surrey.ac.uk/SCRIBA/ndf/(Ion Beam DataFur- nace). (d) http://www.ee.surrey.ac.uk/SCRIBA/ndf/publist.html (publications re RBS simulations). (e) http://www-iba.bo.imm.cnr.it/(a nice compilation of software for ion-beam analyses)

  79. http://en.wikipedia.org/wiki/Van de Graaff generator. Manysuch systems exist; some examples include: (a) Western Michigan University (http://tesla.physics.wmich.edu/AcceleratorFacility. php?PG=1). (b) Brookhaven National Laboratory (http://tvdg10.phy.bnl.gov/index.html). (c) National Institute of Standards and Technology (NIST, http://physics.nist.gov/Divisions/ Div846/Gp2/graaff.html). (d) Yale University (http://wnsl.physics.yale.edu/)

  80. Also known as forward recoil scattering (FRS) or hydrogen forward scattering (HFS).

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  82. For a very thorough web presentation regarding SIMS see: (a) http://www.eaglabs.com/en-US/presentations/TOFSIMS/Presentation Files/index.html (b) http://www.eaglabs.com/en-US/ research/research.html (other links to SIMS theory, applications, presentations)

  83. For background information and recipes to study a variety of polymers using MALDI, see: http://polymers.msel.nist.gov/maldirecipes/maldi.html

  84. For a thesis that has a nice background on ESI, see: http://www.diva-portal.org/diva/getDocument? urn nbn se uu diva-2605-1 fulltext.pdf

  85. Typically, the majority of secondary ions are ejected from the top two or three monolayers (10-20A˚ ) of the sample.

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  97. Examples of some common forces that may exist between a surface and an AFM tip are Van der Waal, electrostatic, covalent bonding, capillary, and magnetic. In addition to providing information regarding the topography of the surface (constant force mode), forces may be applied to understand the morphology of a surface - for example, to determine the frictional force between the tip and surface, or the elasticity/hardness of a surface feature. For instance, see: Tranchida, D.; Piccarolo, S.; Soliman, M. Macromolecules 2006, 39, 4547, and references therein.

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  106. That is, an AFM probe responds to the average force between the sample surface and a group of tip atoms that are in close proximity to the surface. In order to image individual atoms by SPM, the surface-tip interactions must be limited to the nearest atom(s) on the tip periphery. Hence, an AFM image will not show individual atoms, but rather an average surface, with its ultimate resolution dependent on the sharpness of the tip structure. In contrast, STM is capable of atomic resolution since the tunneling current passes only through the tip atom that is nearest the sample surface.

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  109. Tandem TGA/DSC instruments are commercially available, for example: http://www.tainst.com/product.aspx?n=1&id=22

  110. An analogous (older) technique is known as differential thermal analysis (DTA), which yields the same information as DSC.

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  112. Schematics (a) and (b) were obtained from the public domain from the website: http://en.wikipedia.org/wiki/Differentialscanningcalorimetry

  113. For a nice example that utilizes SAXS, WAXS, and SANS to determine the structural changes of polyethylene chains following annealing, see: Men, Y.; Rieger, J.; Lindner, P.; Enderle, H. -F.; Lilge, D.; Kristen, M. O.; Mihan, S.; Jiang, S. J. Phys. Chem. B 2005, 109, 16650.

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  2. Williams, D. B.; Carter, C. B. Transmission Electron Microscopy: A Textbook for Materials Science, Plenum Press: New York, 1996.

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  5. Encyclopedia of Materials Characterization - Surfaces, Interfaces, Thin Films, Brundle, C. R.; Evans, C. A.; Wilson, S. eds., Elsevier: New York, 1992.

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  7. Criddle, W. J.; Ellis, G. P. Spectral and Chemical Characterization of Organic Compounds: A Lab- oratory Handbook, 3rd ed., Wiley: New York, 1990.

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  9. Surface Characterization: A User’s Sourcebook, Brune, D.; Hellborg, R.; Hunderi, O. eds., Wiley: New York, 1997.

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  10. Beam Effects, Surface Topography, and Depth Profiling in Surface Analysis (Methods of Surface Characterization), Czanderna, A. W.; Madey, T. E.; Powell, C. J. eds., Plenum Press: New York, 1998.

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  11. Ion Spectroscopies for Surface Analysis (Methods of Surface Characterization), Czanderna, A. W.; Hercules, D. M. eds., Springer: New York, 1991.

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  12. Brandon, D. D.; Kaplan, W. D. Microstructural Characterization of Materials, Wiley: New York, 1999.

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  13. Pecharsky, V.; Zavalij, P. Fundamentals of Powder Diffraction and Structural Characterization of Materials, Springer: New York, 2005.

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  14. Concise Encyclopedia of Materials Characterization, 2nd ed., Cahn, R. ed., Elsevier: San Diego, CA, 2005.

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  15. Characterization of Polymers (Materials Characterization), Tong, H. -M.; Kowalczyk, S. P.; Saraf, R.; Chou, N. J. eds., Butterworth-Heinemann: New York, 1993.

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Fahlman, B.D. (2007). Materials Characterization. In: Materials Chemistry. Springer, Dordrecht. https://doi.org/10.1007/978-1-4020-6120-2_7

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