Insights: Social Science, Education and Humanities and Characterization... · 2020-04-21 · Insights: Social Science, Education and Humanities Volume1 Issue 2 Insights: Social Science,

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G. Sivagaami Sundaria*, S.Raghub and R.A. Kalaivanic aDepartment of Nanoscience and Technology,

Alagappa University, Karaikudi-630003, bVels Advanced Energy Research Centre, Vels University, Chennai

-117. cDepartment of Chemistry, School of Basic Sciences, Vels University, Chennai -117.

*Corresponding Author Email: [email protected]

Abstract

In research fields dealing with small and micro-molecules, nano-porous carbons are extremely promising

materials. Nonetheless, modern hard and soft design techniques for manufacturing them pose significant

disadvantages linked to high costs of models and sizes. Here, in the combination of carbonation and direct

pyrolysis activation of the biomaterial as a precursor (bamboo bagasse) without use of any chemical

triggering agent, we note the combination of activated carbon material with highly developed nano-porosity

pore volumes. Bamboo bagasse (BB), an organic biomass, has been used without any chemical triggering

agents to produce cheap nano-porous activated carbon. This wood waste has improved the surface properties

by various chemical methods. Surface morphology and surface function groups also play an important role in

the adsorption properties. The aim of this study is to find out the changes occurring in the BB during

activation with carbonization and direct pyrolysis method. Synthesis of activated carbon from BB was

performed as a function of the temperature under Carbon-di-oxide (CO2) flow. A series of experiments have

been conducted to study the effects of different carbonization temperature (600 oC, 700 oC, 800 oC and

900oC) on characteristics of porosity in activated carbon derived from BB. The results showed that the

activated carbon derived from high carbonized temperature of BB, had higher yield with lower ash content,

high specific capacitance, greater graphitic nature. Activated carbon was physically prepared from the

carbonization of BB and its later activation with CO2 and steam of water. Percentage of yields and loss (burn

off) were also evaluated to optimize the experimental operating temperature. Different physical

characterizations were employed to characterize the obtained nanoporous activated carbon from BB. Fourier

Transform Infra-Red (FT-IR) spectroscopy was used for the identification of carbonyls, alkenes, hydroxyl

and other functional groups in the BB. Field Emission Scanning Electron Microscope (FE-SEM) was

employed to show the morphologies of the activated carbon which showed the gradual formation of pores by

Synthesis and Characterization of nanoporous activated

carbon produced from biomass (bamboo bagasse) generation.

Sankardeva

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eliminating the volatile and other contaminants present in it. And also, it is used to find out the adsorptive

capacity of the as-prepared carbon materials. Powder X-Ray Diffraction (XRD) study was carried out to

reveal the amorphous structures with the appearance of the broad diffraction peak. The proximate and

ultimate analysis showed high percentage of carbon with low percentage of ash content which is a indicative

sign of a good material for the production of nanoporous carbon. The present result suggests that waste

biomass is potential source for the synthesis of activated carbon materials with potential novel applications.

Keywords: activated carbon, physical activation, pyrolysis, agricultural wastes, optimum conditions,

characterization

1. Introduction

During the last few decades, development of novel alternatives and technologies which reduces the

environmental pollution at nominal cost and low leave have been developing. The alternatives for the

implementations are granular activated carbon, powdered activated carbon and activated carbon fibers [1].

Nano-porous materials have been traditionally employed in wide range of applications such as catalysis,

adsorption, gas and energy storage devices, optics and electronics. Although the synthesis of carbon

materials with an ordered porous structure in the nanoporous region is highly desirable [2]. Activated carbons

which are usually prepared from the organic matters are very rich and high in carbon content. AC having

high specific porosity, high surface area is extremely versatile adsorbents of major industrial significance [3].

Hence, agricultural waste or the biomass is made an interesting and innovative choice to produce AC with

low and nominal cost and it becomes the biodegradable source. Activated Carbons (AC) are made from

materials that are very enough and rich in carbon content by two different process such as carbonization and

activation [4]. By activation process, the porous structure of the carbon and its adsorption properties can be

achieved. Pyrolysis of the substance source at a temperature of 800oC-1000°C to produce charcoal is the

result of physical activation. This process is then followed by activation using steam or different gas

atmospheres such as carbon-di-oxide (CO2), oxygen (O2). Etc., Activated carbons are one of the called “new

materials” and due to its intrinsic characteristics are widely used in various range of application such as

operation air conditioning systems, creation of personal protection and in the chemical industry [6]. There is

a remarkable interest in producing activated carbon because of its intrinsic properties like adsorptive, eco-

friendly, and also due their good and higher thermal, electrical and mechanical properties. ACs are the most

interesting and commonly leading industrial material because of their well-developed pore structure and





good adsorption properties. In various new AC applications, recent modern technological developments have

shown. The choice of precursors depends in large part on their quality, costs and purity, but also on the

process of production and planned use of the drug [7]. Many other field by-products have been used as

sources of triggering in recent years. Because of the low-price quality, abundance and renewable resources of

agricultural biomass waste it proved to be attractive raw materials to generate activated carbon. AC are

produced from agricultural biomass including rice husk, grape seed, rambutan peel, kena fiber, maize cob,

date bit, coconut shell. Due to its high carbon content, high adsorption capacity, high density and high

mechanical strength, they are employed in the production of AC. In the past, scientists have focused mainly

on the production of industrial waste activated carbon as an alternative to chemically used carbon approach

in the large-scale production field.The lignocelluloses are the most common precursor materials to obtain AC

of low and nominal cost.

AC can be manufactured from several precursors, including wood, farm waste, coal and synthetic

resins. The main aim of this work is to treat bamboo bagasse with a synthesis of carbon materials with the

intention of upgrading biomass fiber. Bamboo bagasse has the following compositions such as cellulose (45-

50%), hemicellulose (20-25%), lignin (20-30%) and some extractives (2.5-5%). A possible solving of this

BB waste is converting it into a value-added AC, which is one of the commonly used materials due to its

awesome adsorbent properties [3]. Due to their excellent natural structure and low ash content, Bamboo

Bagasse (BB) is suitable for AC preparations. BB is a bamboo by-product obtained after the processing of

fruit. Conversion to active carbon can be utilized to reduce cost of waste disposal and provide a relatively

cheap alternative to conventional synthetic carbons as adsorbents, an ion exchange, a carbon molecular sieve

and a catalyst. Studies on CO2 activation of BB have not been reported in literature and hence the present

study attempts to prepare activated carbon with well-developed nano-porosity. Generally, the manufacturing

process of AC involves two different processes such as, carbonization of carbonaceous raw materials in the

presence of the inert gas atmosphere which is then followed by activation of the carbonized product [8].

Hence, the objective of the present study is to synthesize AC from the bamboo bagasse by carbonization

and activation through direct pyrolysis and to optimize the temperature of the experimental condition with

good and higher quantity and quality yield. The aim of this work is to use BB as an activating agent to

prepare activated carbon through physical activation by using CO2 gas. In the preparation of the activated

carbon there are several important factors that influence its composition, including the temperature of

carbonization. In order to achieve high adsorption and surface areas of the drug, the effect on the physi-co-





chemical composition of the activated carbon has also been observed. Due to reduced energy consumption,

capital costs, time production that can boost the economic cycle dramatically, the single-stage physical

activation process with CO2 gas is preferable [9]. The discussion about the influence of gaseous atmosphere

and temperature of the reaction on the texture are also presented. In this study, AC derived from BB by

different processes in analyzed with various techniques such as Scanning Electron Microscope (SEM),

Fourier Transform Infra-Red (FTIR) spectroscopy in order to understand and reveal the properties [10].

2. Experimental Methodology

2.1. Materials required

The following apparatus was used in the course of the research, weighing balance, Muffle furnace,

Beakers, Pestle and Crucible, Thermometer, Filter paper, Funnels, FTIR (Buck 530 FTIR), SEM

(HitachiS-4800), Measuring cylinder, Petri dish.

2.2. Raw Materials and Sample Preparation

The bamboo bagasse was obtained from Bombay hemp company Pvt. Ltd, Bombay. To order to avoid all

the moisture content therein, the raw materials were subsequently washed using hot-distilled water and

dried for about 1 day in a hot-air oven at about 100oC.

2.3 Carbonization of bamboo bagasse

Figure 1. Schematic representation of carbonization of bamboo bagasse

The carbonization of the precursor BB is kept in the muffle furnace under inert atmosphere in the

ambient temperature at 300oC for about 2 hours under a closed system. The schematic representation of

the carbonization process is depicted figure1. After it is cooled, the obtained carbon powder is then





crushed and weighed. The percentage of yield and loss has been calculated [11]. Table.1. represents the

series of experiments of the carbonization process.

Table.1. Tabular representation of carbonization of bamboo bagasse.

Sample.

No.

Sample

Weight (g)-

Before

treatment

Temperature

(oC)

Time (Hours)

Sample Weight

(g)-After

Treatment

Loss in weight

(%)

1. 50.87 250 3 22.61 56.52

2. 50.00 250 3 21.67 56.66

3. 45.00 250 3 22.68 49.6

4. 50.00 250 3 23.09 53.82

5. 50.47 250 3 19.83 60.7

6. 50.02 250 3 17.69 64.63

7 48.67 300 2 21.23 56.37

8. 45.35 300 2 33.61 25.88

9. 42.05 300 2 30.38 27.75

10. 45.55 300 2 33.16 27.2

11. 49.99 300 2 34.36 31.26

12. 40.43 300 2 28.2 30.24

2.3. Activation of bamboo bagasse carbon





Figure 2. Schematic representation of activation set-up and activation process

The figure 2 represents the scheme of the activation set-up and representation of the activation

process. The prepared carbon was then treated into tubular furnace. The carbon was finely

crushed and weighed in a boat crucible and kept into tubular furnace at different temperatures

with flow of different gas atmosphere such as carbon di oxide, argon, hydrogen and nitrogen.

The entire carbonization or activation cycle in this procedure is conducted and other remnants of

components such as oxygen, water, -CH2 are totally burned or vaporized and thus a fully active

carbon sample is collected. The percentage of loss and the yield percentage of the activated

carbon was then calculated. Table 2 represents the series of experiments of activation of bamboo

bagasse carbon.

Table.2. Tabular representation of activation of bamboo bagasse carbon

Sample.

No

Sample Weight

Before Treatment (g)

Temp (oC) Time

(Hours)

After Treatment

Sample

weight(g)

Loss in weight

(%)

Gas Atmosphere

1. 66.85 600 2 1.92 97.12 CO2





2. 68.22 700 2 2.07 96.96 CO2

3. 68.60 900 2 0.38 99.44 CO2

4. 68.26 800 2 1.61 97.64 CO2

5. 68.49 800 6 3.70 94.59 CO2

6. 68.61 800 10 3.70 94.31 CO2

7. 85.90 900 2 10.98 87.21 CO2

8. 68.53 900 2 2.59 96.22 N2

9. 71.73 920 2 4.05 94.35 CO2

10. 68.47 900 2 3.30 95.18 CO2

11. 71.71 900 2 3.48 95.14 CO2

12. 69.89 900 2 2.95 95.77 CO2

13. 100.98 900 2 6.77 93.29 CO2

14. 132.0 900 2 2.55 98.06 CO2

15. 131.94 900 2 8.64 93.45 CO2

16. 130.56 900 2 7.61 94.17 CO2

17. 129.68 850 2 6.4 95.06 CO2

18. 128.70 800 2 4.67 96.37 CO2

19. 130.60 800 3 4.65 96.43 CO2

20. 130.42 800 6 7.13 94.53 CO2

21. 134.62 800 2 7.03 94.77 CO2/10% Urea.

22. 131.06 900 1 4.06 96.90 CO2



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2.4. Physical and Chemical Characterization

2.4.1. FESEM analysis

HitachiS-4800 Electron Microscope was the focus of a morphological study of raw bamboo bagasse.

The instruments have been fitted with double-sided electrically conducting carbon adhesive tabs on a

FESEM holder to avoid damage to the electron beam on the surface of the specimens. The samples were

then coated in a sheet of 20 nm thick gold with a polar-limited E500, a 1.2 kV (10mA) voltage and a 10-

minute vacuum of 20 pa. [12].

2.5.2. Powdered X-ray diffraction study

To create the crystallinity or amorphic structure, XRD was performed. The test was performed using

Cu-Kα radiation source (= 0.15406 Å) with a voltage of 40 kV and a current of 25 mA from Brukers D2

Pheser X-ray diffractometer. The angle of diffraction (2 volts) was between 10o and 90o. With a

scanning rate of 4.2oC / min, radio-diffration patterns were obtained [13].

2.5.3. FTIR spectrum study

Surface chemistry was analyzed using the Fourier transform infrared spectroscopy (FTIR-2000, Perkin

Elmer), to classify the surface functional groups of the samples. In the mid-infrared region, the

spectrums were measured with a resolution of 4000 to 500 cm-1.

3. Result and Discussion

3.1. X-ray Diffraction Studies

The X-Ray Diffraction (XRD) studies is used for the identification of phase of a crystalline material and

gives information about the unit cell dimension. The activated biomass-derived nanoporous carbon of

different temperature was employed for the XRD studies. Figure (3) corresponds to the XRD spectra of

bamboo bagasse-derived nanoporous carbon of different temperatures. Compared to all the other carbon,

the activated nanoporous carbon at 900oC shows two peaks at plane (002) and (101) between the range

26-300 which corresponds to the partial graphitic nature and its better crystalline property. From these

results, it is expected that, as the temperature increases the graphitic nature increases (i.e.) the

temperature and the graphitic nature of the carbon is thus directly proportional to each other [14].



9


Figure 3. XRD analysis of bamboo bagasse derived carbon at different temperatures

3.2. Scanning Electron Microscope

Figure 4 (a,b) SEM images of 900oC/CO2 treated bamboo derived carbon

SEM is a type of electron microscope that images a sample by scanning it with a high-energy beam of

electrons in scan pattern. The electrons interact with the atoms that make up the sample producing signals

that contain information about the sample's surface topography, composition, and other properties such as

electrical conductivity. To determine and examine the morphological structure of the biomass-derived

nanoporous carbon materials scanning electron microscopy (SEM) was employed. HitachiS-4800 field

emission scanning electron microscope is employed for the SEM analysis. Figure 4(a, b) represents low and

high magnification of SEM micrographs of the bamboo bagasse-derived nanoporous carbon sample

900oC/CO2 treated and it is very clear and confident from the figure that the biomass- generation of carbon

leads to the formation of wrinkled discrete sheet with curly form like morphologies with porous cavities in

sparse. The images shows the presence of pores in the 3D interconnected linked together in the carbon

framework. Further, the pores or the voids formation assisted on the decomposition of volatile matter. This

proves that the biomass-derived nanoporous carbon has the approximal resembles of graphene and hence it



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is said to have the partially graphitic nature. This type of resemblance structure would be favorable and can

be employed as an alternative electrode for the energy storage devices since it has been established the

porosity and wrinkled morphology of the commercial graphene materials that governs its energy storage and

power delivery capability [15-17].

3.3. Raman Spectroscopy

Figure 5. Raman spectra of 900oC/CO2 treated bamboo bagasse derived carbon

Figure 5 corresponds to the raman spectra of 900oC/CO2 bamboo bagasse derived nanoporous carbon. In

order to investigate the structure of the biomass-derived nanoporous carbon, Raman analysis was carried

out. This technique was employed because the analysis efficiently characterizes the carbon material as the

raman scattering closely relates to the electronic structure of the materials. The raman spectrum shows two

bands, D & G band. The D band is formed by the degree of disorder and it is called as the defect band. The

G band is formed by the stretching of C-C bond and it represents the graphitic nature of the materials

analyzed. Here, the raman spectrum of the carbon shows D band at ∼1320/cm and G band peak ∼ 1600/cm

respectively. The peaks found near 1000/cm is due to the presence of natural impurities. The 2D peak is also

found near ∼2500/cm and they are due to the resonant processes and it is the secondary peak. In general, the

2D peak will be with larger intensity and shows broader peak for the multi-layered graphene. Here, it show

the broader peak of 2D and it is due to the multi-layered graphene sheet. The peaks obtained are more or

less approximate to the raman spectrum of the commercial graphene. Hence, it can be concluded that the

biomass- derived as-prepared nanoporous carbon has the partially graphitic nature. Since the D band is

higher than the G band, it is to be conformed that the as-prepared nanoporous carbon from biomass has the

amorphous nature in higher range. The Ic/Ig ratio was calculated and found to be 0.99 which represents the

low graphitic crystalline structure [18-21].

4. Conclusion

This work addressed the processing of active carbon as triggering agent, using carbon dioxide. Activated

carbon was prepared from bamboo bagasse by physical activation and pyrolysis under CO2 flow and steam



11


of water. There are optimum times and temperatures which gives conducive results. The carbonization

temperature was determined to significantly influence the porosity of the activated carbon from bamboo

bagasse. The high carbonization temperature (900oC) generated highly nanoporous carbon and the low

carbonization temperatures (600, 700, 800oC) produces did not produce or produces nanoporous carbon.

SEM photographs clearly show differences in the surface morphology between bamboo bagasse and

bamboo bagasse, demonstrating the surface area increase and pores growth after carbonization. After

activation, the FTIR spectroscopy showed that the peak frequencies of functional groups were significantly

different. The XRD results confirmed the reduced crystalline nature and width due to amorphous nature of

the as-prepared activated carbon. It is concluded that, a novel activates carbon can be conveniently and

economically prepared from bamboo bagasse. Thus the as-prepared nanoporous carbon reveals the high

specific capacitance and efficient rate capability for high-performance electro-chemical electrical double

layer capacitor. Generally, the natural biomass derived carbon is highly porous in nature. The biomass

provides 10-14% of world’s energy supply. It is concluded that, among different experimental temperature,

900oC was more efficient with higher quantity and quality yield. Among different gas atmosphere, carbon-

di-oxide was found to be more efficient. The as-prepared biomass derived 900oC/CO2 nanoporous carbon

has partial graphitic nature. The prepared nanoporous carbon reveals the high-specific capacity and high-

performance electro-chemical dual-layer condenser rates.

References:

1. Giraldo, L., Ladino, Y., Pirajánc, J. C., & Rodríguez, M. P. (2007). Synthesis and characterization of activated carbon fibers from

Kevlar. Eclética Química, 32(4), 55-62.

2. Juárez-Galán, J. M., Silvestre-Albero, A., Silvestre-Albero, J., & Rodríguez-Reinoso, F. (2009). Synthesis of activated carbon with

highly developed “mesoporosity”. Microporous and Mesoporous Materials, 117(1-2), 519-521.

3. Gunasekaran, S. S., Elumalali, S. K., Kumaresan, T. K., Meganathan, R., Ashok, A., Pawar, V., ... & Bose, R. S. (2018). Partially

graphitic nanoporous activated carbon prepared from biomass for supercapacitor application. Materials Letters, 218, 165-168.

4. Shamsuddin, M. S., Yusoff, N. R. N., & Sulaiman, M. A. (2016). Synthesis and characterization of activated carbon produced from

kenaf core fiber using H3PO4 activation. Procedia Chemistry, 19, 558-565.

5. Zhuravlev, V. A., Naiden, E. P., Minin, R. V., Itin, V. I., Suslyaev, V. I., & Korovin, E. Y. (2015). Radiation-thermal synthesis of W-

type hexaferrites. In IOP Conference Series: Materials Science and Engineering (Vol. 81, No. 1, p. 012003). IOP Publishing.

6. Juan Matos, Carol Nahas, Laura Rojas, Maibelin Rosales, (2011), Synthesis and characterization of activated carbon from sawdust of

Algarroba wood.1. physical activation and pyrolysis, Journal of Hazardous Materials 196, 360-369.

7. Buasri, A., Chaiyut, N., Loryuenyong, V., Phakdeepataraphan, E., Watpathomsub, S., & Kunakemakorn, V. (2013). Synthesis of

activated carbon using agricultural wastes from biodiesel production. Int J Chem Nucl Mater Metall Eng, 7(1), 98-102.



12


8. J.Raffiea Baseri, P.N.Palanisamy, P.Sivakumar, (2102), Preparation and Characterization of activated carbon from Thevetia Peruviana

for the removal of dyes from textile waste water. Advances in Applied Science Research, 3 (1), 377-383.

9. Abugu, H. O., Okoye, P. A. C., Ajiwe, V. I. E., Omuku, P. E., & Umeobika, U. C. (2015). Preparation and characterization of

activated carbon produced from oil bean (Ugba or Ukpaka) and snail shell. Journal of Environmental Analytical Chemistry, 2(2).

10. Choy, K. K., Barford, J. P., & McKay, G. (2005). Production of activated carbon from bamboo scaffolding waste—process design,

evaluation and sensitivity analysis. Chemical Engineering Journal, 109(1-3), 147-165.

11. Gunasekaran, S. S., Bose, R. S., & Raman, K. (2019). Electrochemical Capacitive Performance of Zncl2 Activated Carbon Derived

from Bamboo Bagasse in Aqueous and Organic Electrolyte. Oriental Journal of Chemistry, 35(1), 302-307.

12. Tang, W., Zhang, Y., Zhong, Y., Shen, T., Wang, X., Xia, X., & Tu, J. (2017). Natural biomass-derived carbons for electrochemical

energy storage. Materials Research Bulletin, 88, 234-241.

13. Peter McKendry, (2002) Energy production from biomass (part 1): overview of biomass, Bioresource Technology 83: 37-46.

14. Peter McKendry, (2002) Energy production from biomass (part 2): conversion technologies, Bioresource Technology 83: 47-54.

15. Deng, J., Li, M., & Wang, Y. (2016). Biomass-derived carbon: synthesis and applications in energy storage and conversion. Green

Chemistry, 18(18), 4824-4854.

16. Wu, X. L., Wen, T., Guo, H. L., Yang, S., Wang, X., & Xu, A. W. (2013). Biomass-derived sponge-like carbonaceous hydrogels and

aerogels for supercapacitors. ACS nano, 7(4), 3589-3597.

17. Wang, H., Li, Z., & Mitlin, D. (2014). Tailoring Biomass‐Derived Carbon Nanoarchitectures for

High‐PerformanceSupercapacitors. ChemElectroChem, 1(2), 332-337.

18. Pozio, A. D., De Francesco, M., Cemmi, A., Cardellini, F., & Giorgi, L. (2002). Comparison of high surface Pt/C catalysts by cyclic

voltammetry. Journal of power sources, 105(1), 13-19.

19. Peter McKendry, (2002) Energy production from biomass (part 3): gasification technology, Bioresource Technology 83: 55-63.

20. Demirbaş, A. (2001). Yields of hydrogen-rich gaseous products via pyrolysis from selected biomass samples. Fuel, 80(13), 1885-

1891.

21. Encinar, J. M., Gonzalez, J. F., & Gonzalez, J. (2002). Steam gasification of Cynara cardunculus L.: influence of variables. Fuel

Processing Technology, 75(1), 27-43.

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Insights: Social Science, Education and Humanities and Characterization... · 2020-04-21 · Insights: Social Science, Education and Humanities Volume1 Issue 2 Insights: Social Science,