Molecular deformation of single spruce wood fibres followed by Raman microscopy

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1 Molecular deformation of single spruce wood fibres followed by Raman microscopy Notburga Gierlinger, Michaela Eder and Ingo Burgert Max-Planck Institute of Colloids and Interfaces Department of Biomaterials Johannes Kepler University Linz Institute of Polymer Science

2 AIM AIM AND APPROACH changes on the molecular level during - tensing - changing environment better understanding of the micromechanics and cell wall polymer properties APPROACH tensile testing of wood tissues and single fibres + Raman microscopy

3 RAMAN EFFECT SIR CHANDRASEKHARA VENKATA RAMAN Rayleigh Scatter (elastic, same wavelength as incident light) Raman Scatter (inelastic, new wavelength)

4 RAMAN- and IR- spectroscopy Virtual hυ 0 h(υ 0 -υ 1 ) h(υ 0 +υ 1 ) excited state ground state 1 0 hυ 1 IR Rayleigh Stokes Anti-Stokes RAMAN ABSORPTION change in dipolmoment SCATTERING change in polarisability

5 RAMAN- and IR- spectroscopy wood spectra OH arom C-C, C-O Raman Intensity Absorbance CH Raman FT-IR cm -1

6 Effect of orientation on Raman band intensity of wood spectra Raman Intensity [CCD cts] red = 0, 3, 6, 9 pink = 12, 15, 18, 21 turkis = 24, 27, 30, 33 blue = 36, 39, 42, 45 light green= 48, 51, 54, 57 green = 60, 63, 66, 69 grey = 72, 75, 78, 81 black = 84, 87, 90, latewood single fibre (MFA<10 ) wavenumber [cm -1 ] Gierlinger, N; Luss, S.; König, Ch.; Konnerth, J.; Eder, M.; Fratzl, P Cellulose microfibril orientation of Picea abies and its variability on the micron-level determined by Raman imaging. Journal of Experimental Botany: in print

7 Prediction of cellulose orientation by band height ratios y= y 0 +ax+bx 2 R 2 Std Err y 0 a b PRESS 1122/ / / Gierlinger, N; Luss, S.; König, Ch.; Konnerth, J.; Eder, M.; Fratzl, P Cellulose microfibril orientation of Picea abies and its variability on the micron-level determined by Raman imaging. Journal of Experimental Botany: in print

8 Prediction of cellulose orientation by PLS models factor R 2 (CAL ) R 2 (CV) RMSECV R 2 (TS) RMSEP Gierlinger, N; Luss, S.; König, Ch.; Konnerth, J.; Eder, M.; Fratzl, P Cellulose microfibril orientation of Picea abies and its variability on the micron-level determined by Raman imaging. Journal of Experimental Botany: in print

9 Prediction of cellulose orientation by Raman compared to X-ray sample layer MFA x-ray 1377/ / / 1095 PLS_3 PLS_1 mean latewood (LW00) S2 rad S2 tang S1 tang S1 rad latewood (LW20) opposite (OW) wood S2 tang S1 tang S2 tang S1 tang compression wood (CW) S2 tang S1 tang Gierlinger, N; Luss, S.; König, Ch.; Konnerth, J.; Eder, M.; Fratzl, P Cellulose microfibril orientation of Picea abies and its variability on the micron-level determined by Raman imaging. Journal of Experimental Botany: in print

10 Effect of tensile load on the Raman spectra low and high stress level) A 1602 Raman Intensity [CCD cts] arom. aryl str. lignin OH cellulose C-C, C-O wavenumber [cm -1 ] Gierlinger, N.; Schwanninger, M.; Reinecke, A.; Burgert, I. 2006: Molecular changes during tensile deformation of single wood fibers followed by Raman microscopy. Biomacromolecules, 7 (7):

11 Gierlinger, N.; Schwanninger, M.; Reinecke, A.; Burgert, I. 2006: Molecular changes during tensile deformation of single wood fibers followed by Raman microscopy. Biomacromolecules, 7 (7): Effect of tensile load on the Raman spectra low and high stress level) B Raman Intensity [CCD cts] wavenumber [cm -1 ]

12 Position and Intensity of the Raman bands is influenced by Composition of the sample (lignin, cellulose, hemicelluloses, extractives) Orientation of the molecules within the sample in respect to the laser polarisation direcetion Status (load) and environment (Dry wet) of the sample APPROACH tensile testing of wood tissues and single fibres + Raman microscopy Stress and reorientation on the molecular level

13 TENSILE TESTER load cell motor water reservoir fibre

14 SPRUCE LATEWOOD: tissue vs single fibre

15 SPRUCE LATEWOOD: tissue vs single fibre Gierlinger, N., Burgert, I. 2006: Secondary cell wall polymers studied by Confocal Raman microscopy: Spatial distribution, orientation and molecular deformation. New Zealand Journal of Forestry Science, 36 (1): 60-71

16 SINGLE SPRUCE FIBRES adult and juvenile latewood 1.4 adult juvenile MFA~5 stress [GPa] MFA~ strain [-]

17 SINGLE SPRUCE FIBRES adult and juvenile latewood latewood juvenile wood 1098 latewood juvenile wood wavenumber [cm -1 ] b[0] = b[1] = r ² = 0.95 wavenumber [cm -1 ] b[0] = b[1] = r ² = strain [-] b[0] = b[1] = r ² = b[0] = b[1] = r ² = stress [GPa]

18 SINGLE SPRUCE FIBRES adult and juvenile - earlywood and latewood adult latewood juvenile latewood MFA~5 1.4 MFA~ LW21 JW5 JW05_0 05 stress [GPa] adult earlywood juvenile earlywood 0.2 EW strain [ ]

19 SINGLE SPRUCE FIBRES adult and juvenile - earlywood and latewood wavenumber [cm -1 ] adult juvenile adult early adult late juv late juv early wavenumber [cm -1 ] earlywood latewood adult early adult late juv late juv early strain [-] MFA stress [GPa] Geometry?

20 SINGLE SPRUCE FIBRES juvenile latewood: dry-wet 100 TENS STOP TENS STOP TENS force [mn] H wavenumber [cm -1 ] time [s]

21 SINGLE SPRUCE FIBRES juvenile latewood: dry-wet 100 TENS STOP TENS STOP TENS TENS STOP TENS STOP TENS force [mn] H wavenumber force [mn] [cm -1 ] H MFA [ ] time [s] cellulose load time [s] microfibril orientation

22 CONCLUSIONS Much higher shifts (loads) in single fibre than in wood tissues Molecular cellulose load correlates across different samples (juvenile, adult, tissue, fibre) with macroscopic stress.except earlywood Monitoring changes in molecular load and orientation simultaneously Wetting of the fibre: Load release through swelling induced change in orientation?

23 ...and you for your ATTENTION THANKS Biomaterial group (MPI Golm) Financial support: Max Planck Society Austrian Academy of Sciences (APART programme) Ingo Burgert Michaela Eder Peter Fratzl

24 INTITUTE OF POLYMER SCIENCE (Head: Prof. Sabine Hild) Polymeric materials Flow characteristics rheology Solidification characteristics crystallization Microstructural characterization with respect to material properties Biological materials Microstructure, local chemical composition and mechanical properties Mineralized tissues, plant cell wall cotton linter cotton linter microtomy, light microscopy Raman-microscopy combined with AFM (PFM) AFM, nanointendation Extruder, Spin coater, DSC, Rheometer Raman AFM

25

26 Samples under load RAMIE single fibre stress [GPa] wavenumber [cm-1} shift [cm-1] cm 1381cm 1095cm 997cm 896cm 459cm 380cm 3378cm OH str strain [] strain change in stress strain curve change in the hydrogen network change in load distribution gliding of fibrils shift [cm-1] cm (HCC, HCO, HOC bending) 1095cm (COC) glycosid 459cm (CCO) ring 380cm (CCC) ring strain

27 Polymer composition and orientation in plant fibres RAMIE 0/0 (parallel) 90/90 0/90 90/0

28 Polymer composition and orientation in plant fibres Ramie fiber 0/0 90/90 0/90 90/ R 1 = I (0/90) /I (0/0) = 0.07 R 2 = I (90/0) /I (90/90) = 0.53 Depolarisation ratios Bacterial cellulose film R 1 = 0.19 R 2 = 0.2 Order parameters P2 and P4 Probable orientation distribution function

29 MOLECULAR DEFORMATION IN WOOD STUDIED BY RAMAN MICROSCOPY Wiley and Atalla (1987) Agarwal and Ralph (1997)

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