Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals

Kazi M. Zakir Hossain; Vincenzo Calabrese; Marcelo A. da Silva; Julien Schmitt; Saffron J. Bryant; Md Towhidul Islam; Reda M. Felfel; Janet L. Scott; Karen J. Edler

doi:10.1002/mame.202000462

Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals

Kazi M. Zakir Hossain^*, Vincenzo Calabrese, Marcelo A. da Silva, Julien Schmitt, Saffron J. Bryant, Md Towhidul Islam, Reda M. Felfel, Janet L. Scott, Karen J. Edler

^*Corresponding author for this work

Mechanical And Aerospace Engineering

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Abstract

In this paper, the microstructural, optical, thermal, crystallization, and water absorption properties of films prepared from never-dried (ND) and freeze-dried (FD) cellulose nanocrystals (CNCs) are reported. Morphology of the ND CNCs reveals a needle-like structure, while after freeze-drying, they show a flake-like morphology. Microstructural analysis of ND and FD CNCs are further studied via small angle X-ray scattering to probe interactions. ND CNCs yield a transparent film with a low surface roughness (14 ± 4 nm), while the FD CNC film evidence a significant reduction of their transparency due to their higher surface roughness (134 ± 20 nm). Although Fourier transform infrared spectroscopy and energy-dispersive X-ray spectroscopy analyses reveal no chemical change occurs during the freeze-drying process, yet a more intense thermal degradation profile is observed for FD CNC film, probably due to the higher oxygen ingress within the gaps created between the stacked flakes. This, in turn, results in a greater loss of crystallinity at a higher temperature (300 °C) compared to the ND CNC film. A rapid decrease in water contact angle of the FD CNC film proves that the morphology of flakes and their orientation within the film has a strong influence in increasing water absorption capacity.

Original language	English
Article number	2000462
Number of pages	12
Journal	Macromolecular Materials and Engineering
Volume	306
Issue number	1
Early online date	23 Nov 2020
DOIs	https://doi.org/10.1002/mame.202000462
Publication status	Published - 15 Jan 2021

Funding

The authors would like to thank EPSRC for funding this project (Grant EP/N033310/1). V.C. thanks the University of Bath for supporting his Ph.D. studies. Prof. Nick Terril, Dr. Andy Smith, and Dr. Tim Snow are thanked for their assistance with SAXS experiment (Experiment no. SM20409-1) at I22 beamline, Diamond Light Source, Didcot, UK. This work benefited from the use of the SasView software (developed under NSF Award DMR-0520547) containing code developed under the EU Horizon 2020 programme (the SINE2020 project Grant 654000). Data supporting this work is freely accessible in the Bath research data archive system at https://doi.org/10.15125/BATH-00930. The authors would like to thank EPSRC for funding this project (Grant EP/N033310/1). V.C. thanks the University of Bath for supporting his Ph.D. studies. Prof. Nick Terril, Dr. Andy Smith, and Dr. Tim Snow are thanked for their assistance with SAXS experiment (Experiment no. SM20409‐1) at I22 beamline, Diamond Light Source, Didcot, UK. This work benefited from the use of the SasView software (developed under NSF Award DMR‐0520547) containing code developed under the EU Horizon 2020 programme (the SINE2020 project Grant 654000). Data supporting this work is freely accessible in the Bath research data archive system at https://doi.org/10.15125/BATH‐00930.

Keywords

cellulose nanocrystals
crystallinity
freeze-drying
thermal degradation
water absorption

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Hossain, K. M. Z., Calabrese, V., da Silva, M. A., Schmitt, J., Bryant, S. J., Islam, M. T., Felfel, R. M., Scott, J. L., & Edler, K. J. (2021). Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals. Macromolecular Materials and Engineering, 306(1), Article 2000462. https://doi.org/10.1002/mame.202000462

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title = "Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals",

abstract = "In this paper, the microstructural, optical, thermal, crystallization, and water absorption properties of films prepared from never-dried (ND) and freeze-dried (FD) cellulose nanocrystals (CNCs) are reported. Morphology of the ND CNCs reveals a needle-like structure, while after freeze-drying, they show a flake-like morphology. Microstructural analysis of ND and FD CNCs are further studied via small angle X-ray scattering to probe interactions. ND CNCs yield a transparent film with a low surface roughness (14 ± 4 nm), while the FD CNC film evidence a significant reduction of their transparency due to their higher surface roughness (134 ± 20 nm). Although Fourier transform infrared spectroscopy and energy-dispersive X-ray spectroscopy analyses reveal no chemical change occurs during the freeze-drying process, yet a more intense thermal degradation profile is observed for FD CNC film, probably due to the higher oxygen ingress within the gaps created between the stacked flakes. This, in turn, results in a greater loss of crystallinity at a higher temperature (300 °C) compared to the ND CNC film. A rapid decrease in water contact angle of the FD CNC film proves that the morphology of flakes and their orientation within the film has a strong influence in increasing water absorption capacity.",

keywords = "cellulose nanocrystals, crystallinity, freeze-drying, thermal degradation, water absorption",

author = "Hossain, {Kazi M. Zakir} and Vincenzo Calabrese and {da Silva}, {Marcelo A.} and Julien Schmitt and Bryant, {Saffron J.} and Islam, {Md Towhidul} and Felfel, {Reda M.} and Scott, {Janet L.} and Edler, {Karen J.}",

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Hossain, KMZ, Calabrese, V, da Silva, MA, Schmitt, J, Bryant, SJ, Islam, MT , Felfel, RM, Scott, JL & Edler, KJ 2021, 'Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals', Macromolecular Materials and Engineering, vol. 306, no. 1, 2000462. https://doi.org/10.1002/mame.202000462

Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals. / Hossain, Kazi M. Zakir; Calabrese, Vincenzo; da Silva, Marcelo A. et al.
In: Macromolecular Materials and Engineering, Vol. 306, No. 1, 2000462, 15.01.2021.

Research output: Contribution to journal › Article › peer-review

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T1 - Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals

AU - Hossain, Kazi M. Zakir

AU - Calabrese, Vincenzo

AU - da Silva, Marcelo A.

AU - Schmitt, Julien

AU - Bryant, Saffron J.

AU - Islam, Md Towhidul

AU - Felfel, Reda M.

AU - Scott, Janet L.

AU - Edler, Karen J.

PY - 2021/1/15

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N2 - In this paper, the microstructural, optical, thermal, crystallization, and water absorption properties of films prepared from never-dried (ND) and freeze-dried (FD) cellulose nanocrystals (CNCs) are reported. Morphology of the ND CNCs reveals a needle-like structure, while after freeze-drying, they show a flake-like morphology. Microstructural analysis of ND and FD CNCs are further studied via small angle X-ray scattering to probe interactions. ND CNCs yield a transparent film with a low surface roughness (14 ± 4 nm), while the FD CNC film evidence a significant reduction of their transparency due to their higher surface roughness (134 ± 20 nm). Although Fourier transform infrared spectroscopy and energy-dispersive X-ray spectroscopy analyses reveal no chemical change occurs during the freeze-drying process, yet a more intense thermal degradation profile is observed for FD CNC film, probably due to the higher oxygen ingress within the gaps created between the stacked flakes. This, in turn, results in a greater loss of crystallinity at a higher temperature (300 °C) compared to the ND CNC film. A rapid decrease in water contact angle of the FD CNC film proves that the morphology of flakes and their orientation within the film has a strong influence in increasing water absorption capacity.

AB - In this paper, the microstructural, optical, thermal, crystallization, and water absorption properties of films prepared from never-dried (ND) and freeze-dried (FD) cellulose nanocrystals (CNCs) are reported. Morphology of the ND CNCs reveals a needle-like structure, while after freeze-drying, they show a flake-like morphology. Microstructural analysis of ND and FD CNCs are further studied via small angle X-ray scattering to probe interactions. ND CNCs yield a transparent film with a low surface roughness (14 ± 4 nm), while the FD CNC film evidence a significant reduction of their transparency due to their higher surface roughness (134 ± 20 nm). Although Fourier transform infrared spectroscopy and energy-dispersive X-ray spectroscopy analyses reveal no chemical change occurs during the freeze-drying process, yet a more intense thermal degradation profile is observed for FD CNC film, probably due to the higher oxygen ingress within the gaps created between the stacked flakes. This, in turn, results in a greater loss of crystallinity at a higher temperature (300 °C) compared to the ND CNC film. A rapid decrease in water contact angle of the FD CNC film proves that the morphology of flakes and their orientation within the film has a strong influence in increasing water absorption capacity.

KW - cellulose nanocrystals

KW - crystallinity

KW - freeze-drying

KW - thermal degradation

KW - water absorption

U2 - 10.1002/mame.202000462

DO - 10.1002/mame.202000462

M3 - Article

AN - SCOPUS:85096715110

SN - 1438-7492

VL - 306

JO - Macromolecular Materials and Engineering

JF - Macromolecular Materials and Engineering

IS - 1

M1 - 2000462

ER -

Microstructural, thermal, crystallization, and water absorption properties of films prepared from never-dried and freeze-dried cellulose nanocrystals

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