Versatile application of a modern scanning electron microscope for materials characterization
Source abstract
Abstract
Abstract Scanning electron microscopy (SEM) is an indispensable characterization technique for materials science. More recently, scanning electron microscopes can be equipped with scanning transmission electron microscopy (STEM) detectors, which considerably extend their capabilities. It is demonstrated in this work that the correlative application of SEM and STEM imaging techniques provides comprehensive sample information on nanomaterials. This is highlighted by the use of a modern scanning electron microscope, which is equipped with in-lens and in-column detectors, a double-tilt holder for electron transparent specimens and a CCD camera for the acquisition of on-axis diffraction patterns. Using multi-walled carbon nanotubes and Pt/Al2O3 powder samples we will show that a complete characterization can be achieved by combining STEM (mass-thickness and diffraction) contrast and SEM (topography and materials) contrast. This is not possible in a standard transmission electron microscope where topography information cannot be routinely obtained. We also exploit the large tilt angle range of the specimen holder to perform 180 degrees STEM tomography on multi-walled carbon nanotubes, which avoids the missing wedge artifacts.
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Research context
OpenAlex topics: Advanced Electron Microscopy Techniques and Applications · Electron and X-Ray Spectroscopy Techniques · Force Microscopy Techniques and Applications
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (31)
Show source-provided references
1. Cowley JM (1969) Image contrast in a transmission scanning electron microscope. Appl Phys Lett 15:58. https://doi.org/10.1063/1.165290110.1063/1.1652901 ↗
2. Bogner A, Jouneau P-H, Thollet G, Basset D, Gauthier C (2007) A history of scanning electron microscopy developments: towards "wet-STEM" imaging. Micron 38:390–401. https://doi.org/10.1016/j.micron.2006.06.00810.1016/j.micron.2006.06.008 ↗
3. Van Ngo V, Hern M, Roth B, Joy DC (2007) STEM imaging of lattice fringes and beyond in a UHR in-lens field-emission SEM. Microscopy Today 15:12–16. https://doi.org/10.1017/S155192950005095110.1017/S1551929500050951 ↗
4. Klein T, Buhr E, Georg Frase C (2012) TSEM: a review of scanning electron microscopy in transmission mode and its applications. Adv Imag Elect Phys 171:297–35610.1016/B978-0-12-394297-5.00006-4 ↗
5. Bell DC, Mankin M, Day RW, Erdman N (2014) Successful application of low voltage electron microscopy to practical materials problems. Ultramicroscopy 145:56–65. https://doi.org/10.1016/j.ultramic.2014.03.00510.1016/j.ultramic.2014.03.005 ↗
6. Guise O, Strom C, Preschilla N (2011) STEM-in-SEM method for morphology analysis of polymer systems. Polymer 52:1278–1285. https://doi.org/10.1016/j.polymer.2011.01.03010.1016/j.polymer.2011.01.030 ↗
7. Drummy LF, Yang J, Martin DC (2004) Low-voltage electron microscopy of polymer molecular thin films. Ultramicroscopy 99:247–256. https://doi.org/10.1016/j.ultramic.2004.01.01110.1016/j.ultramic.2004.01.011 ↗
8. Pfaff M, Klein MFG, Müller E, Müller P, Colsmann A, Lemmer U, Gerthsen D (2012) Nanomorphology of P3HT:PCBM-based absorber layers of organic solar cells after different processing conditions analyzed by low-energy scanning transmission electron microscopy. Microsc Microanal 18:1380–1388. https://doi.org/10.1017/S143192761201344X10.1017/S143192761201344X ↗
9. Kuwajima M, Mendenhall JM, Lindsey LF, Harris KM (2013) Automated transmission-mode scanning electron microscopy (tSEM) for large volume analysis at nanoscale resolution. PLoS ONE 8:e59573. https://doi.org/10.1371/journal.pone.005957310.1371/journal.pone.0059573 ↗
10. Buhr E, Senftleben N, Klein T, Bergmann D, Gnieser D, Frase CG, Bosse H (2009) Characterization of nanoparticles by scanning electron microscopy in transmission mode. Meas Sci Technol 20:084025. https://doi.org/10.1088/0957-0233/20/8/08402510.1088/0957-0233/20/8/084025 ↗
11. Sun C, Müller E, Meffert M, Gerthsen D (2018) On the progress of scanning transmission electron microscopy (STEM) imaging in a scanning electron microscope. Microsc Microanal 24:99–106. https://doi.org/10.1017/S143192761800018110.1017/S1431927618000181 ↗
12. Brodu E, Bouzy E, Fundenberger J-J, Guyon J, Guitton A, Zhang Y (2017) On-axis TKD for orientation mapping of nanocrystalline materials in SEM. Mater Character 130:92–96. https://doi.org/10.1016/j.matchar.2017.05.03610.1016/j.matchar.2017.05.036 ↗
13. Sun C, Müller E, Meffert M, Gerthsen D (2019) Analysis of crystal defects by scanning transmission electron microscopy (STEM) in a modern scanning electron microscope. Adv Struct Chem Imag 5:1. https://doi.org/10.1186/s40679-019-0065-110.1186/s40679-019-0065-1 ↗
14. Casapu M, Fischer A, Gänzler AM, Popescu R, Crone M, Gerthsen D, Türk M, Grunwaldt J-D (2016) Origin of the normal and inverse hysteresis behavior during CO oxidation over Pt/Al2O3. ACS Catal 7:343–355. https://doi.org/10.1021/acscatal.6b0270910.1021/acscatal.6b02709 ↗
15. Leary RK, Midgley PA (2019) Electron tomography in materials science. Springer, Switzerland AG, p 1279
16. Gilbert P (1972) Iterative methods for the three-dimensional reconstruction of an object from projections. J Theor Biol 36:105–117. https://doi.org/10.1016/0022-5193(72)90180-410.1016/0022-5193(72)90180-4 ↗
17. Kremer JR, Mastronarde DN, Mcintosh JR (1996) Computer visualization of three-dimensional image data using IMOD. J Struct Biol 116:71–76. https://doi.org/10.1006/jsbi.1996.001310.1006/jsbi.1996.0013 ↗
18. Mastronarde DN, Held SR (2017) Automated tilt series alignment and tomographic reconstruction in IMOD. J Struct Biol 197:102–113. https://doi.org/10.1016/j.jsb.2016.07.01110.1016/j.jsb.2016.07.011 ↗
19. Howie A (1979) Image contrast and localized signal selection techniques. J Microsc 117:11–23. https://doi.org/10.1111/j.1365-2818.1979.tb00228.x10.1111/j.1365-2818.1979.tb00228.x ↗
20. Hartel P, Rose H, Dinges C (1996) Conditions and reasons for incoherent imaging in STEM. Ultramicroscopy 63:93–114. https://doi.org/10.1016/0304-3991(96)00020-410.1016/0304-3991(96)00020-4 ↗
21. Nellist PD, Pennycook SJ (1999) Incoherent imaging using dynamically scattered coherent electrons. Ultramicroscopy 78:111–124. https://doi.org/10.1016/S0304-3991(99)00017-010.1016/S0304-3991(99)00017-0 ↗
22. Čalkovský M, Müller E, Hugenschmidt M, Gerthsen D (2019) Differential electron scattering cross-sections at low electron energies: the influence of screening parameter. Ultramicroscopy 207:112843. https://doi.org/10.1016/j.ultramic.2019.11284310.1016/j.ultramic.2019.112843 ↗
23. Goudsmit S, Saunderson JL (1940) Multiple scattering of electrons. Phys Rev 57:24–29. https://doi.org/10.1103/PhysRev.57.2410.1103/PhysRev.57.24 ↗
24. Bethe HA, Rose ME, Smith LP (1938) The multiple scattering of electrons. P Am Philos Soc 78:573–585. https://www.jstor.org/stable/984803
25. Konno M, Ogashiwa T, Sunaoschi T, Orai Y, Sato M (2014) Lattice imaging at an accelerating voltage of 30 Kv using an in-lens type cold field-emission scanning electron microscope. Ultramicroscopy 145:28–35. https://doi.org/10.1016/j.ultramic.2013.09.00110.1016/j.ultramic.2013.09.001 ↗
26. Belin T, Epron F (2005) Characterization methods of carbon nanotubes: a review. Mater Sci Eng B 119:105–118. https://doi.org/10.1016/j.mseb.2005.02.04610.1016/j.mseb.2005.02.046 ↗
27. Li M, Yang Y, Huang B, Luo X, Zhang W, Han M, Ru J (2014) Development of advanced electron tomography in materials science based on TEM and STEM. Trans Nonferrous Met Soc China 24:3031–3050. https://doi.org/10.1016/S1003-6326(14)63441-510.1016/S1003-6326(14)63441-5 ↗
28. Ke X, Bals S, Cott D, Hantschel T, Bender H, Van Tendeloo G (2010) Three-dimensional analysis of carbon nanotube networks in interconnects by electron tomography without missing wedge artifacts. Microsc Microanal 16:210–217. https://doi.org/10.1017/S143192760999137110.1017/S1431927609991371 ↗
29. Wang XY, Lockwood R, Malac M, Furukawa H, Meldrum A (2012) Reconstruction and visualization of nanoparticle composites by transmission electron tomography. Ultramicroscopy 113:96–105. https://doi.org/10.1016/j.ultramic.2011.11.00110.1016/j.ultramic.2011.11.001 ↗
30. Li FH, Cheng YF (1990) A simple approach to quasicrystal structure and phasen defect formulation. Acta Cryst A46:142–149. https://doi.org/10.1107/S010876738901132310.1107/S0108767389011323 ↗
31. Sun C, Müller E, Gerthsen D (2019) On the benefits of obtaining surface topography and volume structure information by correlative S(T)EM in a scanning electron microscope. Microsc Microanal 25(S1):73–74. https://doi.org/10.1017/S143192761801609410.1017/S1431927618016094 ↗