Abstract
Developing hemp fibre composites for structural applications requires both reconsideration and optimisation of the transformation processes to obtain stable, high-quality fibre reinforcements. In this context, field retting remains an important issue because it is weather dependent and has not been completely mastered by the hemp industries. Retting can be achieved voluntarily to facilitate fibre separation and extraction from the stalks prior to mechanical decortication. However, retting can also be involuntary and result from climatic misfortune and unforeseeable events at the time of harvest. Therefore, this study aimed to quantify the influence of involuntary and non-controlled field retting on the physicochemical and mechanical properties of industrial hemp bast fibres. A wide spectrum of analytical techniques was applied, including colour spectrophotometry; morphological, microscopic (SEM), surface (EDX, roughness), biochemical (HPLC and pXRD) and thermogravimetric (TGA) analyses; dynamic vapour sorption; and tensile characterisation. The results indicate that retting induced a decrease in the average width of fibre elements after mechanical processing and a loss of pectic substances. We also observed a change in colour from yellow to dark grey, an increase in surface roughness and an increase in the decomposition temperature for the third mass loss region. A decrease in tensile properties at the scales of both single and technical fibres was also observed. Since no significant decrease in cellulose content was measured, this decay in mechanical performance was connected with both the significant degradation of hemicelluloses and a decrease in the fraction of crystalline cellulose that was quantified in this work.
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Abbreviations
- NR-SF:
-
Non-retted single fibres
- NR-TF:
-
Non-retted technical fibres
- R-SF:
-
Retted single fibres
- R-TF:
-
Retted technical fibres
- SF:
-
Single fibres
- TF:
-
Technical fibres
References
Carus M (2015) World-wide market data on hemp and other bast fibres—status and outlook. In: 12th International conference of the European Industrial Hemp Association (EIHA), Wesseling, Germany, May 20th–21st
Carus M, Karst S, Kauffmann A, Hobson J, Bertucelli S (2013) The European Hemp Industry: cultivation, processing and applications for fibres, shivs and seeds. 10th International Conference of the European Industrial Hemp Association (EIHA), Wesseling, Germany, May 22nd–23rd
Bono P, Le Duc A, Lozachmeur M, Day A (2015) Materials: new fields of research and development for the valorization of technical plant fibers (flax fiber and hemp). OCL 22(6):D613
Placet V (2009) Characterization of the thermo-mechanical behaviour of hemp fibres intended for the manufacturing of high performance composites. Compos Part A Appl Sci Manuf 40(8):1111–1118
Placet V, Cisse O, Boubakar ML (2012) Influence of environmental relative humidity on the tensile and rotational behaviour of hemp fibres. J Mater Sci 47:3435–3446. doi:10.1007/s10853-011-6191-3
Duval A, Bourmaud A, Augier L, Baley C (2011) Influence of the sampling area of the stem on the mechanical properties of hemp fibers. Mater Lett 65(4):797–800
Thygesen A (2006) Properties of hemp fibre polymer composites—an optimisation of fibre properties using novel defibration methods and fibre characterisation, PhD Thesis, Risø National Laboratory Roskilde Denmark, p 146
Bourmaud A, Baley C (2007) Investigations on the recycling of hemp and sisal fibre reinforced polypropylene composites. Polym Degrad Stab 92(6):1034–1045
Beckermann GW, Pickering KL (2008) Engineering and evaluation of hemp fibre reinforced polypropylene composites: fibre treatment and matrix modification. Compos Part A Appl Sci Manuf 39(6):979–988
Lu N, Swan RH, Ferguson I (2012) Composition, structure, and mechanical properties of hemp fiber reinforced composite with recycled high-density polyethylene matrix. J Compos Mater 46(16):1915–1924
Madsen B, Thygesen A, Lilholt H (2009) Plant fibre composites - porosity and stiffness. Compos Sci Technol 69(7–8):1057–1069
Thygesen A, Thomsen AB, Daniel G, Lilholt H (2007) Comparison of composites made from fungal defibrated hemp with composites of traditional hemp yarn. Ind Crops Prod 25(2):147–159
Pickering KL, Beckermann GW, Alam SN, Foreman NJ (2007) Optimising industrial hemp fibre for composites. Compos Part A Appl Sci Manuf 38(2):461–468
Shah D (2013) Developing plant fibre composites for structural applications by optimising composite parameters: a critical review. J Mater Sci 48(18):6083–6107. doi:10.1007/s10853-013-7458-7
Rask M, Madsen B, Sörensen BF, Fife JL, Martyniuk K, Lauridsen EM (2012) In situ observations of microscale damage evolution in unidirectional natural fibre composites. Compos Part A Appl Sci Manuf 43(10):1639–1649
Coroller G, Al Lefeuvre, Le Duigou A, Bourmaud A, Ausias G, Gaudry T, Baley C (2013) Effect of flax fibres individualisation on tensile failure of flax/epoxy unidirectional composite. Compos Part A Appl Sci Manuf 51:62–70
Hernandez-Estrada A, Gusovius H-J, Müssig J, Hughes M (2016) Assessing the susceptibility of hemp fibre to the formation of dislocations during processing. Ind Crops Prod 85:382–388
Franck RR (ed) (2005) Bast and other plant fibres. Woodhead Publishing, Boca Raton, USA
Akin DE, Condon B, Sohn M, Foulk JA, Dodd RB, Rigsby LL (2007) Optimization for enzyme-retting of flax with pectate lyase. Ind Crops Prod 25(2):136–146
Ribeiro A, Pochart P, Day A, Mennuni S, Bono P, Baret J-L, Spadoni J-L, Mangin I (2015) Microbial diversity observed during hemp retting. Appl Microbiol Biotechnol 99(10):4471–4484
Sharma HSS, van Sumere CF (1992) The biology and processing of flax. M Publications, Belfast, Northern Ireland
Liu M, Fernando D, Daniel G, Madsen B, Meyer AS, Ale MT, Thygesen A (2015) Effect of harvest time and field retting duration on the chemical composition, morphology and mechanical properties of hemp fibers. Ind Crops Prod 69:29–39
Liu M, Meyer AS, Fernando D, Silva DAS, Daniel G, Thygesen A (2016) Effect of pectin and hemicellulose removal from hemp fibres on the mechanical properties of unidirectional hemp/epoxy composites. Compos A Appl Sci Manuf 90:724–735
Liu M, Silva DAS, Fernando D, Meyer AS, Madsen B, Daniel G, Thygesen A (2016) Controlled retting of hemp fibres: effect of hydrothermal pre-treatment and enzymatic retting on the mechanical properties of unidirectional hemp/epoxy composites. Compos Part A Appl Sci Manuf 88:253–262
Sisti L, Totaro G, Vannini M, Fabbri P, Kalia S, Zatta A, Celli A (2016) Evaluation of the retting process as a pre-treatment of vegetable fibers for the preparation of high-performance polymer biocomposites. Ind Crops Prod 81:56–65
Di Candilo M, Bonatti PM, Guidetti C, Focher B, Grippo C, Tamburini E, Mastromei G (2010) Effects of selected pectinolytic bacterial strains on water-retting of hemp and fibre properties. J Appl Microbiol 108(1):194–203
Di Candilo M, Ranalli P, Bozzi C, Focher B, Mastromei G (2000) Preliminary results of tests facing with the controlled retting of hemp. Ind Crops Prod 11(2–3):197–203
Dreyer J, Müssig J, Koschke N, Ibenthal WD, Harig H (2002) Comparison of enzymatically separated Hemp and Nettle fibre to chemically separated and steam exploded hemp fibre. J Ind Hemp 7(1):43–59. doi:10.1300/J237v07n01_05
Li Y, Pickering KL, Farrell RL (2009) Analysis of green hemp fibre reinforced composites using bag retting and white rot fungal treatments. Ind Crops Prod 29(2–3):420–426
Thygesen A, Liu M, Meyer AS, Daniel G (2013) Hemp fibres: enzymatic effect of microbial processing on fibre bundle structure. In: Risoe international symposium on materials science. Proceedings, 2013. Forskningscenter Risoe Materialeforskning, pp 373–380
Valladares Juarez AG, Dreyer J, Göpel PK, Koschke N, Frank D, Märkl H, Müller R (2009) Characterisation of a new thermoalkaliphilic bacterium for the production of high-quality hemp fibres, Geobacillus thermoglucosidasius strain PB94A. Appl Microbiol Biotechnol 83(3):521–527
Saleem Z, Rennebaum H, Pudel F, Grimm E (2008) Treating bast fibres with pectinase improves mechanical characteristics of reinforced thermoplastic composites. Compos Sci Technol 68(2):471–476
Akin DE, Epps HH, Archibald DD, Sharma HSS (2000) Color measurement of flax retted by various means. Text Res J 70(10):852–858
Berzin F, Vergnes B, Beaugrand J (2014) Evolution of lignocellulosic fibre lengths along the screw profile during twin screw compounding with polycaprolactone. Compos Part A Appl Sci Manuf 59:30–36
Monties B (1984) Dosage de la lignine insoluble en milieu acide: influence du prétraitement par hydrolyse acide sur la lignine Klason de bois et de paille. Agronomie 4(4):387–392
Beaugrand J, Chambat G, Wong VWK, Goubet F, Rémond C, Paès G, Benamrouche S, Debeire P, Donohue MO, Chabbert B (2004) Impact and efficiency of GH10 and GH11 thermostable endoxylanases on wheat bran and alkali-extractable arabinoxylans. Carbohydr Res 339(15):2529–2540
Beaugrand J, Nottez M, Konnerth J, Bourmaud A (2014) Multi-scale analysis of the structure and mechanical performance of woody hemp core and the dependence on the sampling location. Ind Crops Prod 60:193–204
Thygesen A, Oddershede J, Lilholt H, Thomsen AB, Stahl K (2005) On the determination of crystallinity and cellulose content in plant fibres. Cellulose 12(6):563–576
Guicheret-Retel V, Cisse O, Placet V, Beaugrand J, Pernes M, Boubakar ML (2015) Creep behaviour of single hemp fibres. Part II: influence of loading level, moisture content and moisture variation. J Mater Sci 50(5):2061–2072. doi:10.1007/s10853-014-8768-0
Wang HM, Postle R (2004) Improving the color features of hemp fibers after chemical preparation for textile applications. Text Res J 74(9):781–786
Martin N, Mouret N, Davies P, Baley C (2013) Influence of the degree of retting of flax fibers on the tensile properties of single fibers and short fiber/polypropylene composites. Ind Crops Prod 49:755–767
Akin DE (2013) Linen most useful: perspectives on structure, chemistry, and enzymes for retting flax. ISRN Biotechnol 2013:186534. doi:10.5402/2013/186534
Müssig J (2010) Industrial applications of natural fibres: structure, properties and technical applications. doi:10.1002/9780470660324
Virk A (2010) Numerical models for natural fibre composites with stochastic properties, PhD Thesis, University of Plymouth, UK, p 115
Fuentes CA, Brughmans G, Tran LQN, Dupont-Gillain C, Verpoest I, Van Vuure AW (2015) Mechanical behaviour and practical adhesion at a bamboo composite interface: physical adhesion and mechanical interlocking. Compos Sci Technol 109:40–47
George M, Mussone PG, Abboud Z, Bressler DC (2014) Characterization of chemically and enzymatically treated hemp fibres using atomic force microscopy and spectroscopy. Appl Surf Sci 314:1019–1025
Amaducci S, Scordia D, Liu FH, Zhang Q, Guo H, Testa G, Cosentino SL (2015) Key cultivation techniques for hemp in Europe and China. Ind Crops Prod 68:2–16
Fromm J (2010) Wood formation of trees in relation to potassium and calcium nutrition. Tree Physiol 30(9):1140–1147
Hepler PK (2005) Calcium: a central regulator of plant growth and development. Plant Cell 17(8):2142–2155
Akin DE, Henriksson G, Morrison WH, Eriksson K-EL (1998) Enzymatic retting of flax. In: Enzyme applications in fiber processing. ACS symposium series, 687 edn. American Chemical Society, pp 269–278
Willats WT, McCartney L, Mackie W, Knox JP (2001) Pectin: cell biology and prospects for functional analysis. Plant Mol Biol 47(1–2):9–27
Finnan J, Burke B (2013) Potassium fertilization of hemp (Cannabis sativa). Ind Crops Prod 41:419–422
Benito B, Garciadeblás B, Fraile-Escanciano A, Rodríguez-Navarro A (2011) Potassium and sodium uptake systems in fungi. The transporter diversity of Magnaporthe oryzae. Fungal Genet Biol 48(8):812–822
Fischer H, Müssig J (2010) Bast fibre processing and uses. In: Singh B (ed) Industrial crops and uses, p 326
Marrot L, Lefeuvre A, Pontoire B, Bourmaud A, Baley C (2013) Analysis of the hemp fiber mechanical properties and their scattering (Fedora 17). Ind Crops Prod 51:317–327
Jankauskienė Z, Butkutė B, Gruzdevienė E, Cesevičienė J, Fernando AL (2015) Chemical composition and physical properties of dew- and water-retted hemp fibers: Advances in Industrial Crops and Products Worldwide: AAIC 2014 international conference. Ind Crops Prod 75:206–211
Liu M, Fernando D, Meyer AS, Madsen B, Daniel G, Thygesen A (2015) Characterization and biological depectinization of hemp fibers originating from different stem sections. Ind Crops Prod 76:880–891
Blake A, Marcus S, Copeland J, Blackburn R, Knox JP (2008) In situ analysis of cell wall polymers associated with phloem fibre cells in stems of hemp, Cannabis sativa L. Planta 228(1):1–13
Bauer S (2012) Mass spectrometry for characterizing plant cell wall polysaccharides. Front Plant Sci 3:45. doi:10.3389/fpls.2012.00045
Carpita NC, Gibeaut DM (1993) Structural models of primary cell walls in flowering plants: consistency of molecular structure with the physical properties of the walls during growth. Plant J 3(1):1–30
Yasuda S, Fukushima K, Kakehi A (2001) Formation and chemical structures of acid-soluble lignin I: sulfuric acid treatment time and acid-soluble lignin content of hardwood. J Wood Sci 47(1):69–72
Beaugrand J, Berzin F (2013) Lignocellulosic fiber reinforced composites: influence of compounding conditions on defibrization and mechanical properties. J Appl Polym Sci 128(2):1227–1238
Williams PT, Besler S (1993) Thermogravimetric analysis of the components of biomass. In: Bridgwater AV (ed) Advances in thermomechanical biomass conversion, vol 1. Springer, Dordrecht, pp 711–782
Kabir MM (2012) Effects of chemical treatments on Hemp fibre reinforced polyester composite. University of Southern Queensland, Australia
Ouajai S, Shanks RA (2005) Composition, structure and thermal degradation of hemp cellulose after chemical treatments. Polym Degrad Stab 89(2):327–335. doi:10.1016/j.polymdegradstab.2005.01.016
Placet V, Trivaudey F, Cisse O, Gucheret-Retel V, Boubakar ML (2012) Diameter dependence of the apparent tensile modulus of hemp fibres: a morphological, structural or ultrastructural effect? Compos Part A Appl Sci Manuf 43(2):275–287
Virk AS, Hall W, Summerscales J (2010) Failure strain as the key design criterion for fracture of natural fibre composites. Compos Sci Technol 70(6):995–999
Placet V, Cisse O, Boubakar L (2014) Nonlinear tensile behaviour of elementary hemp fibres. Part I: investigation of the possible origins using repeated progressive loading with in situ microscopic observations. Compos Part A Appl Sci Manuf 56:319–327
Placet V, Cisse O, Boubakar ML (2012) Influence of environmental relative humidity on the tensile and rotational behaviour of hemp fibres. J Mater Sci 47(7):3435–3446. doi:10.1007/s10853-011-6191-3
Hill CAS, Norton A, Newman G (2009) The water vapor sorption behavior of natural fibers. J Appl Polym Sci 112(3):1524–1537
Bessadok A, Langevin D, Gouanvé F, Chappey C, Roudesli S, Marais S (2009) Study of water sorption on modified Agave fibres. Carbohydr Polym 76(1):74–85
Acknowledgements
The authors thank Francois Gaudard from FARE for his skilful technical assistance in HPLC, lignin quantification and MEB support. The authors also express theirs thanks to Miguel Pernes for the DVS support. Additionally, Justine Padovani is acknowledged for her critical discussion. Roland Salut, Thomas Jeannin and Paul Tourneroche from FEMTO-ST are thanked for their assistance in energy-dispersive X-ray spectroscopy, surface roughness measurements and ATG, respectively, and Virginie Moutarlier from UTINAM is acknowledged for performing XRD measurements. The authors would also like to thank La Chanvrière Company in France for supplying the hemp fibres. Johnny Beaugrand acknowledges the financial support from the CPER MATRICE state-to-country France-Champagne-Ardenne programme.
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Placet, V., Day, A. & Beaugrand, J. The influence of unintended field retting on the physicochemical and mechanical properties of industrial hemp bast fibres. J Mater Sci 52, 5759–5777 (2017). https://doi.org/10.1007/s10853-017-0811-5
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DOI: https://doi.org/10.1007/s10853-017-0811-5