Skip to main content
SpringerLink
Log in

3D Evaluation of Porous Zeolite Absorbents Using FIB-SEM Tomography

  • Regular Paper
  • Published:
International Journal of Precision Engineering and Manufacturing-Green Technology Aims and scope Submit manuscript

Abstract

An accurate characterization of the microstructure is of great importance in manufacturing zeolites for their appropriate use and optimal performance. Here, an analytical methodology suitable for the complex porous structures of zeolites using focused ion beam (FIB) and scanning electron microscopy (SEM) tomography is demonstrated. For this analysis, a commercial zeolite absorbent is chosen, which is composed of a single zeolite bead filled with small internal beads, like eggs in a brood pouch. Some of the internal zeolite beads and their surrounding pore structures have been precisely reconstructed as three-dimensional (3D) image forms over the micro-scale through FIB-SEM, and the microstructural properties such as particle/pore sizes, specific volume, and surface area are numerically evaluated from the image analysis. This study describes the details of the characterization process from sample preparation to image analysis and discusses major factors influencing the results.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. Weckhuysen, B. M. and Yu, J., “Recent Advances in Zeolite Chemistry and Catalysis,” Chemical Society Reviews, Vol. 44, No. 20, pp. 7022–7024, 2015.

    Article  Google Scholar 

  2. Chue, K., Kim, J., Yoo, Y., Cho, S., and Yang, R., “Comparison of Activated Carbon and Zeolite 13X for CO2 Recovery from Flue Gas by Pressure Swing Adsorption,” Industrial & Engineering Chemistry Research, Vol. 34, No. 2, pp. 591–598, 1995.

    Article  Google Scholar 

  3. Jänchen, J., Ackermann, D., Stach, H., and Brösicke, W., “Studies of the Water Adsorption on Zeolites and Modified Mesoporous Materials for Seasonal Storage of Solar Heat,” Solar Energy, Vol. 76, No. 1, pp. 339–344, 2004.

    Article  Google Scholar 

  4. Cavenati, S., Grande, C. A., and Rodrigues, A. E., “Adsorption Equilibrium of Methane, Carbon Dioxide, and Nitrogen on Zeolite 13X at High Pressures,” Journal of Chemical & Engineering Data, Vol. 49, No. 4, pp. 1095–1101, 2004.

    Article  Google Scholar 

  5. Brandenberger, S., Kröcher, O., Tissler, A., and Althoff, R., “The State of the Art in Selective Catalytic Reduction of NOx by Ammonia Using Metal-Exchanged Zeolite Catalysts,” Catalysis Reviews, Vol. 50, No. 4, pp. 492–531, 2008.

    Article  Google Scholar 

  6. Dong, A., Wang, Y., Tang, Y., Ren, N., Zhang, Y., et al., “Hollow Zeolite Capsules: A Novel Approach for Fabrication and Guest Encapsulation,” Chemistry of Materials, Vol. 14, No. 8, pp. 3217–3219, 2002.

    Article  Google Scholar 

  7. Hwang, Y. K., Chang, J. S., Park, S. E., Kim, D. S., Kwon, Y. U., et al., “Microwave Fabrication of MFI Zeolite Crystals with a Fibrous Morphology and their Applications,” Angewandte Chemie International Edition, Vol. 44, No. 4, pp. 556–560, 2005.

    Article  Google Scholar 

  8. Ma, Y., Tong, W., Zhou, H., and Suib, S. L., “A Review of Zeolite-Like Porous Materials,” Microporous and Mesoporous Materials, Vol. 37, No. 1, pp. 243–252, 2000.

    Article  Google Scholar 

  9. Li, J., Chang, H., Ma, L., Hao, J., and Yang, R. T., “Low-Temperature Selective Catalytic Reduction of NOx with NH3 Over Metal Oxide and Zeolite Catalysts-A Review,” Catalysis Today, Vol. 175, No. 1, pp. 147–156, 2011.

    Article  Google Scholar 

  10. Li, Y. and Yang, W., “Microwave Synthesis of Zeolite Membranes: A Review,” Journal of Membrane Science, Vol. 316, No. 1, pp. 3–17, 2008.

    Article  Google Scholar 

  11. Wang, X., Yang, W., Tang, Y., Wang, Y., Fu, S., et al., “Fabrication of Hollow Zeolite Spheres,” Chemical Communications, No. 21, pp. 2161–2162, 2000.

    Article  Google Scholar 

  12. Lee, W. and Prinz, F. B., “Localized Charge Transfer Reactions Near the Pt-YSZ Interfaces Using Kelvin Probe Microscopy,” Int. J. Precis. Eng. Manuf.-Green Tech., Vol. 1, No. 3, pp. 201–205, 2014.

    Article  Google Scholar 

  13. Kim, S. K., Sung, G., Gwon, J. G., and Kim, J. H., “Controlled Phase Separation in Flexible Polyurethane Foams with Diethanolamine Cross-Linker for Improved Sound Absorption Efficiency,” Int. J. Precis. Eng. Manuf.-Green Tech., Vol. 3, No. 4, pp. 367–373, 2016.

    Article  Google Scholar 

  14. Leamy, H., “Charge Collection Scanning Electron Microscopy,” Journal of Applied Physics, Vol. 53, No. 6, pp. R51–R80, 1982.

    Article  Google Scholar 

  15. Provis, J. L., Myers, R. J., White, C. E., Rose, V., and Van Deventer, J. S., “X-Ray Microtomography Shows Pore Structure and Tortuosity in Alkali-Activated Binders,” Cement and Concrete Research, Vol. 42, No. 6, pp. 855–864, 2012.

    Article  Google Scholar 

  16. Cho, M. K., Youn, H., Jang, S. Y., Lee, S., Han, M.-C., et al., “Digital Tomosynthesis in Cone-Beam Geometry for Industrial Applications: Feasibility and Preliminary Study,” Int. J. Precis. Eng. Manuf., Vol. 13, No. 9, pp. 1533–1538, 2012.

    Article  Google Scholar 

  17. Sheen, D. M., Mc Makin, D. L., and Hall, T. E., “Three-Dimensional Millimeter-Wave Imaging for Concealed Weapon Detection,” IEEE Transactions on Microwave Theory and Techniques, Vol. 49, No. 9, pp. 1581–1592, 2001.

    Article  Google Scholar 

  18. Seo, Y. B., Yun, Y. H., and Joo, K.-N., “3D Multi-Layered Film Thickness Profile Measurements Based on Photometric Type Imaging Ellipsometry,” Int. J. Precis. Eng. Manuf., Vol. 17, No. 8, pp. 989–993, 2016.

    Article  Google Scholar 

  19. Bae, D., Lee, J., Lee, S., Jung, K., Hwang, S., et al., “Nondestructive Evaluation on Hydrogen Effect of 316 l Stainless Steel,” Int. J. Precis. Eng. Manuf.-Green Tech., Vol. 3, No. 1, pp. 99–103, 2016.

    Article  Google Scholar 

  20. Roh, H. D., Lee, H., and Park, Y.-B., “Structural Health Monitoring of Carbon-Material-Reinforced Polymers Using Electrical Resistance Measurement,” Int. J. Precis. Eng. Manuf.-Green Tech., Vol. 3, No. 3, pp. 311–321, 2016.

    Article  Google Scholar 

  21. Uchic, M. D., Holzer, L., Inkson, B. J., Principe, E. L., and Munroe, P., “Three-Dimensional Microstructural Characterization Using Focused Ion Beam Tomography,” MRS Bulletin, Vol. 32, No. 5, pp. 408–416, 2007.

    Article  Google Scholar 

  22. Bilegt, E., Yoon, H.-S., Lee, H.-T., Kim, E.-S., Kim, C.-S., et al., “Design and Evaluation of Micro-Cutting Tools for Local Planarization,” Int. J. Precis. Eng. Manuf., Vol. 17, No. 10, pp. 1267–1273, 2016.

    Article  Google Scholar 

  23. Wilson, J. R., Kobsiriphat, W., Mendoza, R., Chen, H.-Y., Hiller, J. M., et al., “Three-Dimensional Reconstruction of a Solid-Oxide Fuel-Cell Anode,” Nature Materials, Vol. 5, No. 7, pp. 541–544, 2006.

    Article  Google Scholar 

  24. Iwai, H., Shikazono, N., Matsui, T., Teshima, H., Kishimoto, M., et al., “Quantification of SOFC Anode Microstructure Based on Dual Beam FIB-SEM Technique,” Journal of Power Sources, Vol. 195, No. 4, pp. 955–961, 2010.

    Article  Google Scholar 

  25. Volkert, C. A. and Minor, A. M., “Focused Ion Beam Microscopy and Micromachining,” MRS Bulletin, Vol. 32, No. 5, pp. 389–399, 2007.

    Article  Google Scholar 

  26. Gasser, P., Klotz, U. E., Khalid, F. A., and Beffort, O., “Site-Specific Specimen Preparation by Focused Ion Beam Milling for Transmission Electron Microscopy of Metal Matrix Composites,” Microscopy and Microanalysis, Vol. 10, No. 2, pp. 311–316, 2004.

    Article  Google Scholar 

  27. Ali, M. Y., Hung, W., and Yongqi, F., “A Review of Focused Ion Beam Sputtering,” Int. J. Precis. Eng. Manuf., Vol. 11, No. 1, pp. 157–170, 2010.

    Article  Google Scholar 

  28. Uchic, M. D., Groeber, M. A., Dimiduk, D. M., and Simmons, J., “3D Microstructural Characterization of Nickel Superalloys Via Serial-Sectioning Using a Dual Beam FIB-SEM,” Scripta Materialia, Vol. 55, No. 1, pp. 23–28, 2006.

    Article  Google Scholar 

  29. Groeber, M., Haley, B., Uchic, M., Dimiduk, D., and Ghosh, S., “3D Reconstruction and Characterization of Polycrystalline Microstructures Using a FIB-SEM System,” Materials Characterization, Vol. 57, No. 4, pp. 259–273, 2006.

    Article  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. School of Mechanical Engineering, Korea University, 145, Anam-ro, Seongbuk-gu, Seoul, 02841, Republic of Korea

    Kiho Bae, Jun Woo Kim & Joon Hyung Shim

  2. High-temperature Energy Materials Research Center, Korea Institute of Science and Technology, 5, Hwarang-ro 14-gil, Seongbuk-gu, Seoul, 02792, Republic of Korea

    Kiho Bae & Ji-won Son

  3. Nanomaterials Science and Engineering, Korea University of Science and Technology, Korea Institute of Science and Technology, 5, Hwarang-ro 14-gil, Seongbuk-gu, Seoul, 02792, Republic of Korea

    Ji-won Son

  4. Department of Mechanical Science and Engineering, University of Illinois Urbana-Champaign, 1200 W Harrison Street, Chicago, 61801, USA

    Tonghun Lee

  5. Hanchang, 227-14, Amsogogae-ro, Yanggam-myeon, Hwaseong-si, Gyeonggi-do, 18635, Republic of Korea

    Sangkyun Kang

  6. Department of Mechanical Engineering, Stanford University, 450 Serra Mall, Stanford, California, 94305, USA

    Fritz B. Prinz & Joon Hyung Shim

  7. Department of Material Science and Engineering, Stanford University, 450 Serra Mall, Stanford, California, 94305, USA

    Fritz B. Prinz

Authors
  1. Kiho Bae
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Jun Woo Kim
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Ji-won Son
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Tonghun Lee
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Sangkyun Kang
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Fritz B. Prinz
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Joon Hyung Shim
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Joon Hyung Shim.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Bae, K., Kim, J.W., Son, Jw. et al. 3D Evaluation of Porous Zeolite Absorbents Using FIB-SEM Tomography. Int. J. of Precis. Eng. and Manuf.-Green Tech. 5, 195–199 (2018). https://doi.org/10.1007/s40684-018-0019-4

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s40684-018-0019-4

Keywords

Search

Navigation