Raman spectroscopy combines a prominent surface selectivity and an exceptional sensitivity to the degree of structural order (Ashworth et al., 2014). (2016). NH and AD: conducting Raman analysis. doi: 10.1016/j.fuel.2006.03.021, Ashworth, A. J., Sadaka, S. S., Allen, F. L., Sharara, M. A., and Keyser, P. D. (2014). 9, 246253. (2015). Appl. 60, 10541065. doi: 10.1016/j.biortech.2013.08.135, Lewis, A. D., and Fletcher, T. H. (2013). 44, 12471253. Chem. Res. J. Anal. doi: 10.1021/acs.energyfuels.8b03056, Brassard, P., Godbout, S., Raghavan, V., Palacios, J., Grenier, M., and Zegan, D. (2017). 
10, 55855589. Macroscopically, the samples become very fine powders under ultrasound irradiation and microscopically, acoustic activation causes a structural degradation by opening/creation of new micro-pores as observed from the Figures 1B, 2B, 3B, 4B. Mechanisms of metal sorption by biochars: biochar characteristics and modifications. Renew. Pyrolysis temperature has a prominent role in promoting the ultrasound effect. Similar to raw biochars, sono-chemically functionalized samples exhibited an increasing trend of adsorption capacities with temperature up to 700C, followed by a reduction at 800C; optimum adsorption capacities were obtained for temperatures 600700C, which is in accordance to the Table 3 that showed notable differences (>3% change) in %C contents of MS, SG and SB at 600C temperature. The ratio of the disorder-induced band (D band) to the Raman-allowed band (G band) is termed the intensity ratio (ID/IG). In brief, adsorption experiments were conducted in a temperature-controlled tubular reactor (alumina oxide, Al2O3). As observed, maximum surface area values for both the microporosity (R-SG-700 with surface area 325 m2/g) and micro-mesoporosity (R-SG-800 with surface area 351 m2/g) are observed for herbaceous residues, whereas the minimum values for the microporosity (R-SB-500 with surface area 83 m2/g) and micro-mesoporosity (R-SB-500 with surface area 138 m2/g) are observed for agro-industrial based chars. doi: 10.5539/mas.v9n4p246, Major, I., Pin, J.-M., Behazin, E., Rodriguez-Uribe, A., Misra, M., and Mohanty, A. Fuel 235, 11311145. doi: 10.1002/aic.14347, Chen, Y., Yang, H., Wang, X., Zhang, S., and Chen, H. (2012). The surface area of the samples can be further justified based on the adsorption isotherm plots as observed in the Figures S2, S3. The maximum pore generation was observed for 700C, accordingly SEM images of sonicated chars pyrolyzed at 700C have been presented. Appl. doi: 10.1016/B9780-08087872-0.005242, Brunauer, S., Deming, L. S., Deming, W. E., and Teller, E. (1940). doi: 10.1016/j.petlm.2016.11.001, Verma, Y. L., Singh, M. P., and Singh, R. K. (2012). 141, 8388. doi: 10.1016/j.rser.2014.01.056, Rafiq, M. K., Bachmann, R. T., Rafiq, M. T., Shang, Z., Joseph, S., and Long, R. (2016). In order to prevent misinterpretation concerning organic content, elemental analysis of aminated samples is discussed by eliminating the impact of ash alteration. Sust. Dynamic molecular structure of plant biomass-derived black carbon (biochar). Above 600C, decomposition for all the biochars completed and the curves became stable. Effect of feedstock and pyrolysis temperature on properties of biochar governing end use efficacy. Cu (II) removal from aqueous solution by spartina alterniflora derived biochar. 
SG also exhibit similar behavior where %C content showed gradual increment and %N content showed gradual reducing trend with temperature but C-N peak from IR showed improved intensity for aminated samples at 600 and 700C than raw SG under same temperatures. Technol. Variables governing the initial stages of the synergisms of ultrasonic treatment of biochar in water with dissolved CO2. Elemental compositions (dry basis) of raw and activated biochar samples synthesized at different pyrolysis temperatures. Influence of pyrolysis temperature on production and nutrient properties of wastewater sludge biochar. The results of the present study also generally exhibited enhancement of ash content with pyrolysis temperature, mainly due to the increase in the concentration of minerals (such as Na, Mg, Ca, K, etc.) The sharp peak at the 2 values around 23 associated with the crystalline cellulose for amorphous regions (Figure 8A) (Jiang et al., 2007; Osman et al., 2018). 118, 536544. doi: 10.5539/jas.v5n1p1, Pilon, G., and Lavoie, J.-M. (2013). doi: 10.1021/ja01864a025, Budai, A., Wang, L., Gronli, M., Strand, L. T., Antal, M. J., Abiven, S., et al. Figure 1. Images obtained revealed two main morphological features for all biochar samples: fiber structures and pith. This is mostly attributed to the further degradation of lignin and the reaction of aromatic condensation (Chen et al., 2012), which increases the release of volatile matter and creates more pores. The surface area data can be also verified using the SEM analysis results as observed from Figures 14. Technol. This facility was supported in part by grant 1726880, National Science Foundation. doi: 10.1002/ep.12783, Paris, O., Zollfrank, C., and Zickler, G. A. Cleaner production of iron by using waste macadamia biomass as a carbon resource. Technol. doi: 10.1016/j.still.2015.10.002, Liu, Y., He, Z., and Uchimiya, M. (2015). The surface crystallinity of the biochar samples were determined from the XRD analysis in a Rigaku powder diffractometer (Rigaku, Japan) with Cu K radiation ( = 0.15406 nm). National Science Foundation (NSF EPSCoR RII Grant No. doi: 10.1016/j.biombioe.2014.01.004, Nwajiaku, I. M., Olanrewaju, J. S., Sato, K., Tokunari, T., Kitano, S., and Masunaga, T. (2018). The mass loss occurred slowly around 6070C, which is associated with the loss of the initial moisture of the raw sample observed in Figure 7A (Santos et al., 2015). Sust. The TGA curve for aminated samples (7B) have similar trend as observed for raw samples where the samples showed reduction in mass around 6070C attributed to the desorption of moisture. OIA-1632899 and MRI Grant No. Ind. Org. This trend can be correlated to Tables 2, 3 that showed significant changes in surface areas and elemental compositions, respectively, when pyrolysis temperature was increased from 500 to 600C, irrespective of the biochar type.
Chemosphere 90, 26232630. J. Environ. Removal of ash from the biochar structure could be attributed to the washing away of mineral contents of the biochars during aqueous modifications (Kim W. K. et al., 2013). This structural deformation can be explained because of the thinner walls of CS and SB than MS and SG. 231, 512518. Anal. On a theory of the van der waals adsorption of gases. 5, 18.
Eng. This describes the amount of disorganized material present (Wang S. et al., 2015). This trend is further verified from the following physicochemical characterizations data. 
It can be concluded from the table that the ultrasono-amine functionalized adsorbents which were prepared from miscanthus, switchgrass, cornstover and sugarcane bagasse under 700C have comparatively higher adsorption capacities (2.222.89 mmol/g) than most of the reported data. Energies 5, 49525001. Eng. Int. A new peak at 43 appeared for samples pyrolyzed at 600 and 700C that indicated the development of atomic order in the increasingly carbonized material (Keiluweit et al., 2010).
158, 218224. Solid amine sorbents for CO2 capture by chemical adsorption: a review. 
Appl. Properties of biochar derived from wood and high-nutrient biomasses with the aim of agronomic and environmental benefits. Calorim. 
Energy 37, 10581067. Increasing pyrolysis temperature had a significant effect on the elemental constituents and H/C (the degree of aromaticity) (Al-Wabel et al., 2013) and O/C (the degree of polarity) ratios (Mimmo et al., 2014) of raw biochars. (2008). Technol. Chemosphere 178, 466478. The original IR plots are shown in Figure S1. Bioresour. Pissa: Combustion Institute Italian section. The sonicated samples also showed significant increases in surface area (323 to 520 m2/g for MS, from 309 to 486 m2/g for SG, from 215 to 399 m2/g for CS, and 192332 m2/g for SB) with increasing the pyrolysis temperature from 500 to 600C. The lower the ID/IG ratio, the higher the degree of graphitization of the carbonaceous structure. 118, 158162. This shows that surface area is significantly affected by the biochar feedstock and pyrolysis temperature. Further increase of the temperature to 700C magnifies surface area and pore volume, especially for the micropores. Application of thermogravimetric analysis to the evaluation of aminated solid sorbents for CO2 capture. Thus, biochar samples produced within the temperature range of 500700C showed better reactivity and adsorption behavior than biochar samples produced at 800C.
Chem.
doi: 10.1016/j.biombioe.2015.11.010, Sun, Y., Gao, B., Yao, Y., Fang, J., Zhang, M., Zhou, Y., et al. Based on Figure 9, adsorption capacities for activated chars can be categorized as: 0.861.23, 2.152.53, 2.222.89, and 1.341.74 mmol/g for the temperature ranges of 500, 600, 700, and 800C, respectively. 62, 247258. It must also be highlighted that the activating treatments of the biochars were conducted near room temperature, making the sonication and amination activation processes notably energy efficient, compared to thermal activation. The effect of high power ultrasound on an aqueous suspension of graphite. doi: 10.1016/j.biortech.2012.04.094, Kim, P., Johnson, A. M., Essington, M. E., Radosevich, M., Kwon, W.-T., Lee, S.-H., et al. XRD-thermal combined analyses: an approach to evaluate the potential of phytoremediation, phytomining, and biochar production.
Front. 1, 198204. Evaluation of various types of Al-MCM-41 materials as catalysts in biomass pyrolysis for the production of bio-fuels and chemicals. The use, distribution or reproduction in other forums is permitted, provided the original author(s) and the copyright owner(s) are credited and that the original publication in this journal is cited, in accordance with accepted academic practice. No use, distribution or reproduction is permitted which does not comply with these terms. In addition, the most notable change in the ID/IG intensity ratio of both herbaceous and agro-industrial chars was observed when the temperature was raised from 500 to 600C followed by a slight increment from 600 to 800C. Most of the biochars showed intensified peak at 1,4001,600 cm1 attributed to aromatic C=C stretching except for MS. doi: 10.1016/S1001-0742(13)60421-0, Zhang, L., Gonalves, A. The maximum adsorption capacities and the highest level of adsorption increment upon acoustic-based amination were both observed at 600700C, which were 2.83.1 times greater than the adsorption capacity of the corresponding raw biochars.
doi: 10.1021/jf501139f, Cetin, E., Gupta, R., and Moghtaderi, B. doi: 10.1016/j.jaap.2011.11.010, Inyang, M., Gao, B., Pullammanappallil, P., Ding, W., and Zimmerman, A. R. (2010). Notably, higher pyrolysis temperatures gave rise to the peak at 23 consistent to the literature (Kim et al., 2012). (2017). However, its intensity was typically reduced at higher temperatures. A., and Jaroniec, M. (2020). The present study investigated the importance of pyrolysis temperature on biochar properties, acoustic-based amination of biochar, and CO2 adsorption. The surface area and pore volume (both micro and micro-meso porosity) of raw and ultrasound activated samples pyrolyzed under different temperatures are reported in Table 2. doi: 10.1016/j.ultsonch.2009.08.011, Hagemann, N., Spokas, K., Schmidt, H.-P., Kgi, R., Bhler, M., and Bucheli, T. (2018). 
This could be due to the reduction in surface area at elevated temperature (800C) caused by the destruction of surface porosity, in addition to the reduction in %N contents at 800C (Tables 2, 3). (2013). (2014). As a result of the addition of disordered functional groups, the ID/IG intensity ratio is expected to be greater for sono-aminated chars compared with raw samples. But a further increase in pyrolysis temperature (to 800C) resulted in a reduction in %C content and similarly follows a reverse trend for other elemental constituents. A comprehensive review on physical activation of biochar for energy and environmental applications. doi: 10.1515/revce-20180003, Santos, L. B., Striebeck, M. V., Crespi, M. S., Ribeiro, C. A., and De Julio, M. (2015). Generally, the minimum CO2 capture was observed in agro-industrial category, particularly SB biochar. Similar observations are found in the literature and in our previous studies (Stankovich et al., 2006; Chen et al., 2014; Chatterjee et al., 2018, 2019; Sajjadi et al., 2019a). Energies 7, 548567. Consistent with this, almost all activated biochars (except A-SG-600/700 and A-SB-700/800) demonstrated a significant increase in the ID/IG ratio compared with their pristine condition (Table S2). Production, characterization and reactivity studies of chars produced by the isothermal pyrolysis of flax straw. Also aminated SB samples such as A-SB 500 and A-SB 700 have enhanced C-N peak than R-SB 500 and R-SB 700. Nature 442, 282286. Ultrasound cavitation intensified amine functionalization: a feasible strategy for enhancing CO2 capture capacity of biochar. The D-band is attributed to in-plane vibrations of sp2 bonded carbon (intramolecular CC vibration of aromatic carbon layers) within structural defects (Pilon and Lavoie, 2013). Similar structural features are also observed for CS (Figure 3A) and SB (Figure 4A), which exhibit rough, irregular and bundle like shapes.
For instance, CS follows an increasing trend of %C content up to 700C with a gradual rise of ash content and reduction of H/C and O/C ratios and %N contents.
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