Abstract
Carbon nanofiber (CNF) aerogels are a new class of advanced materials that have many potential applications in the energy and environmental sectors. However, some CNF aerogels consist of materials derived from fossil-fuels and energy-intensive production processes. For the successful industry-scale applications of carbon aerogels, the development of large-scale production methods with a smaller environmental footprint is required. Cellulose is a promising alternative material as a precursor of CNF aerogels, due to its renewability, high carbon content, and carbon neutrality. However, the low yield of CNF aerogels from the pyrolysis of cellulose nanofiber (CellNF) aerogels hinders their practical applications. To increase the yield of CNF aerogels from the pyrolysis of CellNF aerogels, we investigated the use of ammonium chloride (NH4Cl) as a carbonization promoter. The influence of the amount of NH4Cl, pyrolysis temperature, and method of adding NH4Cl to the cellulose precursor were systematically studied. Drastic improvements were observed in the yields of CNF aerogels, by 141–446% at 600 °C and 118–225% at 800 °C of pyrolysis, with the addition of NH4Cl (0.5–1.5 NH4Cl/CellNF weight ratio). The morphology, chemical and crystalline characteristics, microstructure, and porosity of CNFs in the aerogels were not affected by the addition of NH4Cl.
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Arteaga-Pérez L, Cápiro O, Delgado A, Martín S (2017) Elucidating the role of ammonia-based salts on the preparation of cellulose-based carbon aerogels. Chem Eng Sci 161:80–91
Balakumar K, Kalaiselvi N (2015) High sulfur loaded carbon aerogel cathode for lithium–sulfur batteries. RSC Adv 5:34008–34018
Brunauer S, Emmett PH, Teller E (1938) Adsorption of gases in multimolecular layers. J Am Chem Soc 60:309–319
Chandrasekaran S, Campbell PG, Baumann TF, Worsley MA (2017) Carbon aerogel evolution: allotrope, graphene-inspired, and 3D-printed aerogels. J Mater Res 32:4166–4185
Chung YK, Koo JH, Kim SA, Chi EO, Hahn JH, Park C (2014) Optimization of reaction parameters for synthesis of amorphous silicon nitride powder by vapor phase reaction. Ceram Int 40:14563–14568
Crombie K, Mašek O (2014) Investigating the potential for a self-sustaining slow pyrolysis system under varying operating conditions. Bioresour Technol 162:148–156
Cuesta A, Dhamelincourt P, Laureyns J, Martinez-Alonso A, Tascón JD (1994) Raman microprobe studies on carbon materials. Carbon 32:1523–1532
Erdey L, Gal S, Liptay G (1964) Thermoanalytical properties of analytical-grade reagents: ammonium salts. Talanta 11:913–940
French AD (2014) Idealized powder diffraction patterns for cellulose polymorphs. Cellulose 21:885–896
Garn PD, Denson CL (1977) Pyrolysis products from cellulose treated with flame retardants: part I: halogen-containing flame retardants. Text Res J 47:485–491
Goto M, Yokoe Y (1996) Ammoniation of barley straw. Effect on cellulose crystallinity and water-holding capacity. Anim Feed Sci Technol 58:239–247
Gupta S, Tai NH (2016) Carbon materials as oil sorbents: a review on the synthesis and performance. J Mater Chem A4:1550–1565
Hao X, Wang J, Ding B, Wang Y, Chang Z, Dou H, Zhang X (2017) Bacterial-cellulose-derived interconnected meso-microporous carbon nanofiber networks as binder-free electrodes for high-performance supercapacitors. J Power Sour 352:34–41
He P, Liu Y, Shao L, Zhang H, Lü F (2018) Particle size dependence of the physicochemical properties of biochar. Chemosphere 212:385–392
Hirata T, Nishimoto T (1991) DSC, DTA, and TG of cellulose untreated and treated with flame-retardants. Thermochim Acta 193:99–106
Hoekstra J, Beale AM, Soulimani F, Versluijs-Helder M, Geus JW, Jenneskens LW (2015) Base metal catalyzed graphitization of cellulose: a combined Raman spectroscopy, temperature-dependent X-ray diffraction and high-resolution transmission electron microscopy study. J Phys Chem C 119:10653–10661
Howarth J, Mareddy SSR, Mativenga PT (2014) Energy intensity and environmental analysis of mechanical recycling of carbon fibre composite. J Clean Prod 81:46–50
Ishida O, Kim D, Kuga S, Nishiyama Y, Malcolm Brown J (2004) Microfibrillar carbon from native cellulose. Cellulose 11:475–480
Jawhari T, Roid A, Casado J (1995) Raman spectroscopic characterization of some commercially available carbon black materials. Carbon 33:1561–1565
Jazaeri E, Tsuzuki T (2013) Effect of pyrolysis conditions on the properties of carbonaceous nanofibers obtained from freeze-dried cellulose nanofibers. Cellulose 20:707–716
Jazaeri E, Zhang L, Wang X, Tsuzuki T (2011) Fabrication of carbon nanofiber by pyrolysis of freeze-dried cellulose nanofiber. Cellulose 18:1481–1485
Kan K, Kim D (2012) Influence of sulfuric acid impregnation on the carbonization of cellulose. Korean Phys Soc 60:1818–1822
Karacan I, Soy T (2013) Enhancement of oxidative stabilization of viscose rayon fibers impregnated with ammonium sulfate prior to carbonization and activation steps. J Appl Polym Sci 128:1239–1249
Keiluweit M, Nico PS, Johnson MG, Kleber M (2010) Dynamic molecular structure of plant biomass-derived black carbon (biochar). Environ Sci Technol 44:1247–1253
Khalil HPSA, Davoudpour Y, Islam MN, Mustaph A, Sudesh K, Dungani R, Jawaid M (2014) Production and modification of nanofibrillated cellulose using various mechanical processes: a review. Carbohydr Polym 99:649–665
Khanna V, Bakshi BR, Lee LJ (2008) Carbon nanofiber production: life cycle energy consumption and environmental impact. J Ind Ecol 12:394–410
Khezami L, Chetouani A, Taouk B, Capart R (2005) Production and characterisation of activated carbon from wood components in powder: cellulose, lignin, xylan. Powder Technol 157:48–56
Kim DY, Nishiyama Y, Wada M, Kuga S (2001) High-yield carbonization of cellulose by sulfuric acid impregnation. Cellulose 8:29–33
Kim KH, Vural M, Islam MF (2011) Single-walled carbon nanotube aerogel-based elastic conductors. Adv Mater 23:2865–2869
Kuga S, Kim DY, Nishiyama Y (2002) Nanofibrillar carbon from native cellulose. Mol Cryst Liq Cryst 387:237–243
Kurnevich GI, Loiko EM, Gert EV, Skoropanov AS, Buyanova VK, Gridina UF (1985) Study of the influence of ammonium salts on the regenerated cellulose thermodestruction. Thermochim Acta 90:335–338
Kuzmenko V, Naboka O, Gatenholm P, Enoksson P (2014) Ammonium chloride promoted synthesis of carbon nanofibers from electrospun cellulose acetate. Carbon 67:694–703
Lee EJ, Lee YJ, Kim JK, Lee M, Yi J, Yoon JR, Song JC, Song IK (2015) Oxygen group-containing activated carbon aerogel as an electrode material for supercapacitor. Mater Res Bull 70:209–214
Li H, Yang Y, Wen Y, Liu L (2007) A mechanism study on preparation of rayon based carbon fibers with (NH4)2SO4/NH4Cl/organosilicon composite catalyst system. Compos Sci Technol 67:2675–2682
Li S, Warzywoda J, Wang S, Ren G, Fan Z (2017) Bacterial cellulose derived carbon nanofiber aerogel with lithium polysulfide catholyte for lithium–sulfur batteries. Carbon 124:212–218
Li S, Hu B, Ding Y, Liang H, Li C, Yu Z, Wu Z, Chen W, Yu S (2018) Wood-derived ultrathin carbon nanofiber aerogels. Ang Chem 11:7203–7208
Ling Z, Wang T, Makarem M, Cintrón MS, Cheng HN, Kang X, Bacher M, Potthast A, Rosenau T, King H, Delhom CD, Nam S, Edwards JV, Kim SH, Xu F, French AD (2019) Effects of ball milling on the structure of cotton cellulose. Cellulose 26:305–328
Lu L, Sahajwalla V, Kong C, Harris D (2001) Quantitative X-ray diffraction analysis and its application to various coals. Carbon 39:1821–1833
Luo W, Schardt J, Bommier C, Wang B, Razink J, Simonsen J, Ji X (2013) Carbon nanofibers derived from cellulose nanofibers as a long-life anode material for rechargeable sodium-ion batteries. J Mater Chem A 1:10662–10666
Ma C, Song Y, Shi J, Zhang D, Zhai X, Zhong M, Guo Q, Liu L (2013) Preparation and one-step activation of microporous carbon nanofibers for use as supercapacitor electrodes. Carbon 51:290–300
Manoj B, Kunjomana AG (2012) Study of stacking structure of amorphous carbon by X-ray diffraction technique. Int J Electrochem Sci 7:3127–3134
Meng Y, Young TM, Liu P, Contescu CI, Huang B, Wang S (2015) Ultralight carbon aerogel from nanocellulose as a highly selective oil absorption material. Cellulose 22:435–447
Meyer DE, Curran MA, Gonzale MA (2009) An examination of existing data for the industrial manufacture and use of nanocomponents and their role in the life cycle impact of nanoproducts. Environ Sci Technol 43:1256–1263
Mittal A, Katahira R, Himmel ME, Johnson DK (2011) Effects of alkaline or liquid-ammonia treatment on crystalline cellulose: changes in crystalline structure and effects on enzymatic digestibility. Biotechnol Biofuels 4:41
Morgan P (2005) Carbon fiber production using a cellulose based precursor. Carbon fibers and their composites. CRC Press, Boca Raton, pp 269–294
Nogi M, Kurosaki F, Yano H, Takano M (2010) Preparation of nanofibrillar carbon from chitin nanofibers. Carbohydr Polym 81:919–924
Oulton D (1995) Fire retardant textiles. In: Carr C (ed) Chemistry of the textiles industry. Chapman & Hall, Glasgow, pp 110–114
Pappa A, Mikedi K, Tzamtzis N, Statheropoulos M (2003) Chemometric methods for studying the effects of chemicals on cellulose pyrolysis by thermogravimetry-mass spectrometry. J Anal Appl Pyrol 67:221–235
Peng S, Shao H, Hu X (2003) Lyocell fibers as the precursor of carbon fibers. J Appl Polym Sci 90:1941–1947
Peng Y, Gardner DJ, Han Y (2011) Drying cellulose nanofibrils: in search of a suitable method. Cellulose 19:91–102
Peng X, Shen S, Wang C, Li T, Li Y, Yuan S, Wen X (2017) Influence of relative proportions of cellulose and lignin on carbon-based solid acid for cellulose hydrolysis. Mol Catal 442:133–139
Poole A, Church J, Huson M (2008) Environmentally sustainable fibers from regenerated protein. Biomacromol 10:1–8
Rhim YR, Zhang D, Fairbrother DH, Wepasnick KA, Livi KJ, Bodnar RJ, Nagle DC (2010) Changes in electrical and microstructural properties of microcrystalline cellulose as function of carbonization temperature. Carbon 48:1012–1024
Rouquerol J, Llewellyn P, Rouquerol F (2007) Is the BET equation applicable to microporous adsorbents? In: Llewellyn P, Rodriguez-Reinoso F, Rouquerol J, Seaton N (eds) Characterization of porous solids VII, Studies in surface science and catalysis. Elsevier, Amsterdam and Oxford, pp 49–56
Sadezky A, Muckenhuber H, Grothe H, Niessner R, Pöschl U (2005) Raman microspectroscopy of soot and related carbonaceous materials: spectral analysis and structural information. Carbon 43:1731–1742
Sawada D, Hanson L, Wada M, Nishiyama Y, Langan P (2014) The initial structure of cellulose during ammonia pretreatment. Cellulose 21:1117–1126
Schultz TP, McGinnis GD, Nicholas DD (1990) Effect of crystallinity and additives on the thermal degradation of cellulose. In: Nelson GL (ed) Fires and polymers. Chapter 22. American Chemical Society, Washington DC, pp 335–360
Segal L, Creely JJ, Martin AE, Conrad CM (1959) An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Tex Res J 29:786–794
Shang H, Lu R, Shang L, Zhang W (2015) Effect of additives on the microwave-assisted pyrolysis of sawdust. Fuel Proc Technol 131:167–174
Song YS, Youn JR, Gutowski TG (2009) Life cycle energy analysis of fiber-reinforced composites. Compos A 40:1257–1265
Steinhauser G (2008) Cleaner production in the solvay process: general strategies and recent developments. J Clean Prod 16:833–841
Stoeckli HF, Kraehenbuehl F, Ballerini L, De Bernardini S (1989) Recent developments in the Dubinin equation. Carbon 27:125–128
Tang S, Sun G, Qi J, Sun S, Guo J, Xin Q, Haarberg GM (2010) Review of new carbon materials as catalyst supports in direct alcohol fuel cells. Chin J Catal 31:12–17
Tao Y, Endo M, Kaneko K (2008) A review of synthesis and nanopore structures of organic polymer aerogels and carbon aerogels. Recent Pat Chem Eng 1:192–200
Thommes M, Kaneko K, Neimark AV, Olivier JP, Rodriguez-Reinoso F, Rouquerol J, Sing KS (2015) Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC technical report). Pure Appl Chem 87:1051–1069
Tushar MS, Mahinpey N, Khan A, Ibrahim H, Kumar P, Idem R (2012) Production, characterization and reactivity studies of chars produced by the isothermal pyrolysis of flax straw. Biomass Bioenergy 37:97–105
Virtanen J, Pammo A, Keskinen J, Sarlin E, Tuukkanen S (2017) Pyrolysed cellulose nanofibrils and dandelion pappus in supercapacitor application. Cellulose 24(8):3387–3397
Wagner EL, Hornig DF (1950) The vibrational spectra of molecules and complex ions in crystals III. Ammonium chloride and deutero-ammonium chloride. J Chem Phys 18:296–304
White RJ, Brun N, Budarin VL, Clark JH, Titirici MM (2014) Always look on the “light” side of life: sustainable carbon aerogels. Chemsuschem 7:670–689
Wu Z, Li C, Liang H, Chen J, Yu S (2013) Ultralight, flexible, and fire-resistant carbon nanofiber aerogels from bacterial cellulose. Angew Chem Int Ed 52:2925–2929
Yen TF, Erdman JG, Pollack SS (1961) Investigation of the structure of petroleum asphaltenes by X-ray diffraction. Anal Chem 33:1587–1594
Zhang L, Tsuzuki T, Wang X (2015) Preparation of cellulose nanofiber from softwood pulp by ball milling. Cellulose 22:1729–1741
Zhang X, Yan Q, Leng W, Li J, Zhang J, Cai Z, Hassan EB (2017) Carbon nanostructure of kraft lignin thermally treated at 500 to 1000 C. Materials 10:975
Zhuang X, Zhan H, Song Y, He C, Huang Y, Yin X, Wu C (2019) Insights into the evolution of chemical structures in lignocellulose and non-lignocellulose biowastes during hydrothermal carbonization (HTC). Fuel 236:960–974
Acknowledgments
We acknowledge the Centre for Advanced Microscopy, Australia National University (ANU) for the use of SEM. Mahdiar Taheri at ANU obtained the SEM images and thermogravimetric data of the samples. We thank Dr. Antonio Tricoli for the use of an XRD and a gas-absorption analyzer; also Dr. Jodie Bradby and Thomas Shiell for the use of a micro-Raman spectrometer. We also recognize the postdoctoral fellowship grant provided by the Engineering Research and Development for Technology, Department of Science and Technology, Philippines.
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Pajarito, B.B., Llorens, C. & Tsuzuki, T. Effects of ammonium chloride on the yield of carbon nanofiber aerogels derived from cellulose nanofibrils. Cellulose 26, 7727–7740 (2019). https://doi.org/10.1007/s10570-019-02645-0
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DOI: https://doi.org/10.1007/s10570-019-02645-0