Skip to main content
Log in

The nanostructure of kraft pulp 1: evaluation of various mild drying methods using field emission scanning electron microscopy

  • Published:
Cellulose Aims and scope Submit manuscript

Abstract

Wood pulp fiber consists of carbohydrate fibrils containing crystalline cellulose microfibrils of a few nanometer width. The structure of the fibril in water is currently unclear due to the difficulty of imaging pulp fiber in water at nanometer resolution. An alternative method is to observe the sample dried with a mild drying method to preserve the structure of the wet sample. In this study, we studied softwood kraft pulp fibers which were dried with various mild drying methods and then imaged by field emission scanning electron microscopy at nanometer resolution. Both mild dried samples, as well as air dried samples, showed 10–20 nm wide fibrils, the width of which corresponded to a crystalline cellulose microfibril or bundles of them. The mild dried sample, which was critical point dried with liquid CO2 (CPD), mainly showed 20–40 nm thick fibrils, in addition to the 10–20 nm fibrils. The existence of the thick fibril implies that the fibril itself has a swelling nature in water, although the possibility that the thick fibril was an artifact of the CPD process could not be excluded. Further investigation as to the extent that the thick fibrils found in the CPD samples reflect the nanostructure of pulp fiber in water is warranted.

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

Access this article

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

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7

Similar content being viewed by others

Abbreviations

FE-SEM:

Field emission scanning electron microscopy

CPD:

Critical point drying with liquid CO2

RFND:

Rapid freezing and normal freeze-drying

TBAFD:

Freeze-drying with t-butyl alcohol

WAD:

Air drying from water

References

  • Abe H, Ohtani J, Fukazawa K (1991) FE-SEM observations on the microfibrillar orientation in the secondary wall of tracheids. IAWA Bull 12:431–438

    Google Scholar 

  • Abe H, Funada R, Ohtani J, Fukazawa K (1995) Changes in the arrangement of microtubules and microfibrils in differentiating conifer tracheids during the expansion of cells. Ann Bot 75:305–310

    Article  Google Scholar 

  • Anderson TF (1950) The use of critical point phenomena in preparing specimens for the electron microscope. J Appl Phys 21:724

    Article  Google Scholar 

  • Daniel G, Duchesne I (1998) Revealing the surface ultrastructure of spruce pulp fibres using field emission-SEM. In: Proceedings 7th International Conference on Biotechnology in the Pulp and Paper Industry, June 16–19, Vancouver, Canada, pp B81–B85

  • Duchesne I, Daniel G (1999) The ultrastructure of wood fibre surfaces as shown by a variety of microscopical methods–a review. Nord Pulp Pap Res J 14:129–139

    Article  CAS  Google Scholar 

  • Duchesne I, Hult E, Molin U, Daniel G, Iversen T, Lennholm H (2001) The influence of hemicellulose on fibril aggregation of kraft pulp fibres as revealed by FE-SEM and CP/MAS C-13-NMR. Cellulose 8:103–111

    Article  CAS  Google Scholar 

  • Frey-Wyssling A (1954) The fine structure of cellulose microfibrils. Science 119:80–82

    Article  CAS  Google Scholar 

  • Hosoo Y, Yoshida M, Imai T, Okuyama T (2002) Diurnal difference in the amount of immunogold-labeled glucomannans detected with field emission scanning electron microscopy at the innermost surface of developing secondary walls of differentiating conifer tracheids. Planta 215:1006–1012

    Article  CAS  Google Scholar 

  • Hult EL, Iversen T, Sugiyama J (2003) Characterization of the supermolecular structure of cellulose in wood pulp fibres. Cellulose 10:103–110

    Article  CAS  Google Scholar 

  • Inoue T, Osatake H (1988) A new drying method of biological specimens for scanning electron microscopy: the t-butyl alcohol freeze-drying method. Arch Histol Cytol 51:53–59

    Article  CAS  Google Scholar 

  • Jayme G, Hunger G (1962) Electron microscope 2- and 3-dimensional classification of fiber bonding. In: Bolam F (ed) The formation and structure of paper. Technical section of the British paper and board makers’ association, London, 1: pp 135-169

  • Kerr AJ, Goring DAI (1975) Ultrastructural arrangement of the wood cell wall. Cellul Chem Technol 9:563–573

    Google Scholar 

  • Kinsinger WG, Hock CW (1948) Electron microscopical studies of natural cellulose fibers. Ind Eng Chem 40:1711–1716

    Article  CAS  Google Scholar 

  • Okamoto T, Meshitsuka G (2003) Determination of the surface layer of kraft pulp fibers by field emission scanning electron microscopy (FE-SEM). J Jpn TAPPI 57:1532–1536

    Google Scholar 

  • Pang L, Gray DG (1998) Heterogeneous fibrillation of kraft pulp fibre surfaces observed by atomic force microscopy. J Pulp Pap Sci 24:369–372

    CAS  Google Scholar 

  • Pelton RH (1993) A model of the external surface of wood pulp fibers. Nord Pulp Pap Res J 8:113–119

    Article  CAS  Google Scholar 

  • Sasaki T, Okamoto T, Meshitsuka G (2006) Influence of deformability of kraft pulp fiber surface estimated by force curve measurements on atomic force microscope (AFM) contact mode imaging. J Wood Sci 52:377–382

    Article  Google Scholar 

  • Scallan AM (1974) The structure of the cell wall of wood-a consequence of anisotropic inter-microfibrillar bonding. Wood Sci 6:266–270

    Google Scholar 

  • Stone JE, Scallan AM (1965) Effect of component removal upon the porous structure of the cell wall of wood. J Polym Sci C: Polym Symp 11:13–25

    Article  Google Scholar 

  • Stone JE, Scallan AM (1967) The effect of component removal pon the porous structure of the cell wall of wood. Part II. Swelling in water and the fiber saturation point. Tappi J 50:496–501

    CAS  Google Scholar 

  • Stone JE, Scallan AM (1968) A structural model for the cell wall of water-swollen wood pulp fibres based on their accessibility to macromolecules. Cellul Chem Technol 2:343–358

    CAS  Google Scholar 

  • Sugiyama J, Harada H, Fujiyoshi Y, Uyeda N (1985) Lattice images from ultrathin sections of cellulose microfibrils in the cell wall of Valonia macrophysa K tz. Planta 166:161–168

    Article  Google Scholar 

  • Wickholm K, Larsson PT, Iversen T (1998) Assignment of non-crystalline forms in cellulose I by CP/MAS C-13 NMR spectroscopy. Carbohydr Res 312:123–129

    Article  CAS  Google Scholar 

Download references

Acknowledgments

We thank Dr. T. Sasaki, Ms. H. Naganuma, Dr. T. Akiyama and Dr. A. Palanisami for critical discussion, Dr. Y. Matsumoto and Dr. T. Yokoyama for their helpful advice and encouragement, and members of Laboratory of Wood Chemistry for help and advice.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Tetsuaki Okamoto.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Okamoto, T., Meshitsuka, G. The nanostructure of kraft pulp 1: evaluation of various mild drying methods using field emission scanning electron microscopy. Cellulose 17, 1171–1182 (2010). https://doi.org/10.1007/s10570-010-9452-4

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10570-010-9452-4

Keywords

Navigation