Startseite Chemical modifications of acid-treated pine needle fillers reinforced epoxy nanocomposites for enhanced thermomechanical properties using a response surface methodology approach: fabrication and optimization
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Chemical modifications of acid-treated pine needle fillers reinforced epoxy nanocomposites for enhanced thermomechanical properties using a response surface methodology approach: fabrication and optimization

  • Manish , Deepak Kumar EMAIL logo , Anil Punia , Lalit Ranakoti EMAIL logo , Brijesh Gangil , Prabhakar Bhandari , Shubham Sharma ORCID logo EMAIL logo und Ehab El Sayed Massoud
Veröffentlicht/Copyright: 25. August 2025

Abstract

This study explores the design and development of chemically modified epoxy nanocomposites reinforced with acid-treated pine needle (PN) fillers, aiming to enhance the mechanical and thermal properties of sustainable materials. The research examines the effects of nitric acid treatment on PN fillers, focusing on improvements in filler adhesion, surface roughness, and contaminant removal. Characterization techniques such as Fourier-transform infrared spectroscopy (FTIR) and Thermogravimetric Analysis (TGA) confirm the chemical modifications and enhanced thermal stability of the treated fillers. FTIR analysis confirmed chemical modifications through enhanced C–O–C and reduced –OH absorption bands. The acid-treated fillers exhibited a density of 1,120 ± 43.42 kg/m3, confirming their suitability for lightweight applications. TGA results indicated improved thermal stability of the acid-treated fillers, with the onset of major degradation delayed from approximately 265 °C in untreated fillers to around 288 °C in treated fillers, and a higher residual weight observed at 600 °C. Epoxy nanocomposites were fabricated using precise filler-epoxy mixing, degassing, and curing processes. Tensile and impact tests, conducted according to ASTM standards, revealed significant improvements in mechanical properties, particularly tensile strength (TS) and impact strength (IS), influenced by filler weight, ultra-sonication time, and degassing time. Response surface methodology (RSM) and analysis of variance (ANOVA) were employed to optimize the composite synthesis process, yielding an optimized composite with a TS of 60.85 MPa and an IS of 14.67 kJ/m2. The optimized composite exhibited a 25 % increase in TS and a 30 % increase in IS compared to neat epoxy. These findings highlight the potential of acid-treated PN fillers in producing high-performance, eco-friendly composites for automotive, aerospace, and construction applications. Future work will explore further optimization and real-world performance testing of these composites.


Corresponding authors: Deepak Kumar, Assistant Professor, Department of Mechanical Engineering, Invertis University, Bareilly, 243123, India, E-mail: ; Lalit Ranakoti, Department of Mechanical Engineering, Graphic Era Deemed to be University, Clementown, Dehradun, Uttarakhand-248002, India, E-mail: ; and Shubham Sharma, Lloyd Institute of Engineering & Technology, Plot No. 3, Knowledge Park II, Greater Noida, Uttar Pradesh 201306, India; Department of Technical Sciences, Western Caspian University, Baku, Azerbaijan; and Jadara University Research Center, Jadara University, Irbid, Jordan, E-mail:

Acknowledgment

The authors extend their appreciation to the Deanship of Research and Graduate Studies at King Khalid University for funding this work through Large Research Project under grant number RGP2/531/45. Secondly, kindly retain both the funding as well as acknowledgment sections in the final online publication of this manuscript, please, as this is an indispensable stuff.

  1. Research ethics: Not applicable.

  2. Informed consent: Not Applicable.

  3. Author contributions: Conceptualization, M, DK, AP, LR, BG, SS; formal analysis, M, DK, AP, LR, BG, PB, SS, SPD; investigation, M, DK, AP, LR, BG, SS; writing – original draft preparation, M, DK, AP, LR, BG, SS; writing – review and editing, PB, SS, EESM; project administration, PB, SS, EESM; funding acquisition, PB, SS, EESM. All authors have read and agreed to the published version of the manuscript. All authors have read and agreed to the published version of the manuscript.

  4. Conflict of interest: The authors declare no competing interests.

  5. Use of Large Language Models, AI and Machine Learning Tools: Not Applicable.

  6. Research funding: The authors extend their appreciation to the Deanship of Research and Graduate Studies at King Khalid University for funding this work through Large Research Project under grant number RGP2/531/45.

  7. Data availability: All the characterizations, analysis, testing’s related works, and testing’s has solely been responsible by Deepak Kumar. Additionally, the raw data can be obtained on request from the main corresponding author, Deepak Kumar. In addition, the datasets used and/or analysed during the current study available from the corresponding author (Deepak Kumar) on reasonable request.

References

[1] G. R. H. Wright, Ancient Building in South Syria and Palestine, Leiden, E.J. Brill, 1985.10.1163/9789004493704Suche in Google Scholar

[2] D. Kumar and A. Mandal, “Predictive analysis of tensile strength ratios in laminated bamboo composites: unraveling the stochastic impact of ply angle variations through machine learning model,” Proc. Inst. Mech. Eng. Part C J. Mech. Eng. Sci., vol. 2024, p. 09544062241277318, 2024.10.1177/09544062241277318Suche in Google Scholar

[3] V. Bahuguna, P. K. Rakesh, A. Mandal, and D. Kumar, “Characterisation of gaina cocoon foam: a promising and eco-friendly alternative to synthetic materials,” Proc. Inst. Mech. Eng. Part C J. Mech. Eng. Sci., vol. 238, no. 6, pp. 1–10, 2023. https://doi.org/10.1177/14644207231216867.Suche in Google Scholar

[4] D. Kumar and A. Mandal, “Review on manufacturing and fundamental aspects of laminated bamboo products for structural applications,” Constr. Build. Mater., vol. 348, p. 128691, 2022. https://doi.org/10.1016/j.conbuildmat.2022.128691.Suche in Google Scholar

[5] K. Obi Reddy, G. Sivamohan Reddy, C. Uma Maheswari, A. Varada Rajulu, and K. Madhusudhana Rao, “Structural characterization of coconut tree leaf sheath fiber reinforcement,” J. For. Res., vol. 21, pp. 53–8, 2010. https://doi.org/10.1007/s11676-010-0008-0.Suche in Google Scholar

[6] T. Thamae and C. Baillie, “Influence of fibre extraction method, alkali and silane treatment on the interface of Agave americana waste HDPE composites as possible roof ceilings in Lesotho,” Compos. Interfaces, vol. 14, no. 7–9, pp. 821–36, 2007. https://doi.org/10.1163/156855407782106483.Suche in Google Scholar

[7] P. G. Baskaran, M. Kathiresan, P. Senthamaraikannan, and S. S. Saravanakumar, “Characterization of new natural cellulosic fiber from the bark of Dichrostachys cinerea,” J. Nat. Fibers, vol. 15, no. 1, pp. 62–8, 2018. https://doi.org/10.1080/15440478.2017.1304314.Suche in Google Scholar

[8] A. Valadez-Gonzalez, J. M. Cervantes-Uc, R. Olayo, and P. J. Herrera-Franco, “Effect of fiber surface treatment on the fiber–matrix bond strength of natural fiber reinforced composites,” Compos. Part B Eng., vol. 30, no. 3, pp. 309–20, 1999. https://doi.org/10.1016/S1359-8368(98)00054-7.Suche in Google Scholar

[9] P. A. Sreekumar, S. P. Thomas, J. marc Saiter, K. Joseph, G. Unnikrishnan, and S. Thomas, “Effect of fiber surface modification on the mechanical and water absorption characteristics of sisal/polyester composites fabricated by resin transfer molding,” Compos. Part A Appl. Sci. Manuf., vol. 40, no. 11, pp. 1777–84, 2009. https://doi.org/10.1016/j.compositesa.2009.08.013.Suche in Google Scholar

[10] V. Raghunathan, et al.., “Influence of chemical treatment on the physico-mechanical characteristics of natural fibers extracted from the barks of Vachellia farnesiana,” J. Nat. Fibers, vol. 9, no. 13, 2021. https://doi.org/10.1080/15440478.2021.1875353.Suche in Google Scholar

[11] L. Y. Mwaikambo and M. P. Ansell, “Chemical modification of hemp, sisal, jute, and kapok fibers by alkalization,” J. Appl. Polym. Sci., vol. 84, no. 12, pp. 2222–34, 2002. https://doi.org/10.1002/app.10460.Suche in Google Scholar

[12] S. J. S. Chelladurai, K. Murugan, A. P. Ray, M. Upadhyaya, V. Narasimharaj, and S. Gnanasekaran, “Optimization of process parameters using response surface methodology: a review,” Mater. Today Proc., vol. 37, no. 2, pp. 1301–4, 2020. https://doi.org/10.1016/j.matpr.2020.06.466.Suche in Google Scholar

[13] D. T. Ebissa, T. Tesfaye, D. Worku, and D. Wood, “Characterization and optimization of the properties of untreated high land bamboo fibres,” Heliyon, vol. 8, no. 8, p. e09856, 2022. https://doi.org/10.1016/j.heliyon.2022.e09856.Suche in Google Scholar PubMed PubMed Central

[14] A. A. Salih, R. Zulkifli, and C. H. Azhari, “Tensile properties of single cellulosic bamboo fiber (Gigantochloa scortechinii) using response surface methodology,” J. Nat. Fibers, vol. 19, no. 1, pp. 359–68, 2022. https://doi.org/10.1080/15440478.2020.1745117.Suche in Google Scholar

[15] M. Z. Hassan, et al.., “Mercerization optimization of bamboo (Bambusa vulgaris) fiber-reinforced epoxy composite structures using a box-behnken design,” Polymers (Basel), vol. 12, no. 6, pp. 1–19, 2020. https://doi.org/10.3390/POLYM12061367.Suche in Google Scholar PubMed PubMed Central

[16] A. S. Singh, S. Halder, J. Wang, and Jagadish, “Extraction of bamboo micron fibers by optimized mechano-chemical process using a central composite design and their surface modification,” Mater. Chem. Phys., vol. 199, no. 0, pp. 23–33, 2017. https://doi.org/10.1016/j.matchemphys.2017.06.040.Suche in Google Scholar

[17] J. Alberch and U. Aut, “Master’s degree final project,” 2018.Suche in Google Scholar

[18] D. Kumar and A. Mandal, “Response surface method-based optimisation of advanced mechanochemical approach for bead minimisation in bamboo fiber extraction, and improving hydrophobicity via diisopropanolamine treatment,” Biomass Convers. Biorefin., vol. 14, 2023. https://doi.org/10.1007/s13399-023-04420-5.Suche in Google Scholar

[19] R. Kumar, P. K. Rakesh, D. Sreehari, D. Kumar, and T. P. Naik, “Experimental investigations on material properties of alkali retted Pinus roxburghii fiber,” Biomass Convers. Biorefin., vol. 14, 2023. https://doi.org/10.1007/s13399-023-04245-2.Suche in Google Scholar

[20] Y. AbouelNour, N. Rakauskas, G. Naquila, and N. Gupta, “Tensile testing data of additive manufactured ASTM D638 standard specimens with embedded internal geometrical features,” Sci. Data, vol. 11, no. 506, pp. 1–6, 2024. https://doi.org/10.1038/s41597-024-03369-y.Suche in Google Scholar PubMed PubMed Central

[21] D. P. A. Santosa and I. Widiastuti, “Suharno. Mechanical properties of bamboo on virgin and recycled high-density polyethylene matrix,” IOP Conf. Ser. Earth Environ. Sci., vol. 1808, no. 2021, pp. 2–8, 2021. https://doi.org/10.1088/1742-6596/1808/1/012009.Suche in Google Scholar

[22] N. G. S. Silva, T. F. Maia, and D. R. Mulinari, “Effect of acetylation with perchloric acid as catalyst in sugarcane bagasse waste,” J. Nat. Fibers, vol. 19, no. 13, pp. 5050–64, 2022. https://doi.org/10.1080/15440478.2021.1875352.Suche in Google Scholar

[23] Y. A. El-Shekeil, S. M. Sapuan, A. Khalina, E. S. Zainudin, and O. M. Al-Shuja’A, “Effect of alkali treatment on mechanical and thermal properties of kenaf fiber-reinforced thermoplastic polyurethane composite,” J. Therm. Anal. Calorim., vol. 109, no. 0, pp. 1435–43, 2012. https://doi.org/10.1007/s10973-012-2258-x.Suche in Google Scholar

[24] M. R. Sanjay, S. Siengchin, J. Parameswaranpillai, M. Jawaid, C. I. Pruncu, and A. Khan, “A comprehensive review of techniques for natural fibers as reinforcement in composites: preparation, processing and characterization,” Carbohydr. Polym., vol. 207, pp. 108–21, 2019. https://doi.org/10.1016/j.carbpol.2018.11.083.Suche in Google Scholar PubMed

[25] L. Sthle and S. Wold, “Analysis of variance (ANOVA),” Chemom. Intell. Lab. Syst., vol. 6, no. 4, pp. 259–72, 1989. https://doi.org/10.1016/0169-7439(89)80095-4.Suche in Google Scholar

[26] S. Sharma, P. Sudhakara, M. Petru, J. Singh, and S. Rajkumar, “Effect of nanoadditives on the novel leather fiber/recycled poly(ethylene-vinyl-acetate) polymer composites for multifunctional applications: fabrication, characterizations, and multiobjective optimization using central composite design,” Nanotechnol. Rev., vol. 11, no. 1, pp. 2366–2432, 2022. https://doi.org/10.1515/ntrev-2022-0067.Suche in Google Scholar

[27] J. M. Khare, et al.., “Comparative analysis of erosive wear behavior of epoxy, polyester and vinyl esters based thermosetting polymer composites for human prosthetic applications using taguchi design,” Polymers, vol. 13, no. 20, p. 3607, 2021, https://doi.org/10.3390/polym13203607.Suche in Google Scholar PubMed PubMed Central

[28] Y. Singh, J. Singh, S. Sharma, V. Aggarwal, and C. I. Pruncu, “Multi-objective optimization of kerf-taper and surface-roughness quality characteristics for cutting-operation on coir and carbon fiber reinforced epoxy hybrid polymeric composites during CO2-pulsed laser-cutting using RSM,” Lasers Manuf. Mater. Process, vol. 8, no. 2, pp. 157–82, 2021, https://doi.org/10.1007/s40516-021-00142-6.Suche in Google Scholar

[29] J. S. Chohan, et al.., “Optimization of FDM printing process parameters on surface finish, thickness, and outer dimension with ABS polymer specimens using Taguchi orthogonal array and genetic algorithms,” Math. Probl. Eng., vol. 2022, no. 1, p. 2698845, 2022, https://doi.org/10.1155/2022/2698845.Suche in Google Scholar

[30] K. Dhanasekar, et al.., “Influences of nanosilica particles on density, mechanical, and tribological properties of sisal/hemp hybrid nanocomposite,” Adv. Polym. Technol., vol. 2023, 2023. https://doi.org/10.1155/2023/3684253.Suche in Google Scholar

[31] C. Balaji Ayyanar, et al.., “Experimental and numerical analysis of natural fillers loaded and E-glass reinforced epoxy sandwich composites,” J. Mater. Res. Technol., vol. 32, pp. 1235–44, 2024. https://doi.org/10.1016/j.jmrt.2024.07.142.Suche in Google Scholar

[32] A. M. Seid and S. A. Adimass, “Review on the impact behavior of natural fiber epoxy based composites,” Heliyon, vol. 10, no. 20, p. e39116, 2024. https://doi.org/10.1016/j.heliyon.2024.e39116.Suche in Google Scholar PubMed PubMed Central

[33] T. A. Nguyen and T. H. Nguyen, “Banana fiber-reinforced epoxy composites: mechanical properties and fire retardancy,” Int. J. Chem. Eng., vol. 2021, 2021. https://doi.org/10.1155/2021/1973644.Suche in Google Scholar

[34] S. Nath, H. Jena, and S. D. Priyanka, “Analysis of mechanical properties of jute epoxy composite with cenosphere filler,” Silicon, vol. 11, pp. 659–71, 2019. https://doi.org/10.1007/s12633-018-9941-x.Suche in Google Scholar

Received: 2025-01-14
Accepted: 2025-07-16
Published Online: 2025-08-25

© 2025 Walter de Gruyter GmbH, Berlin/Boston

Heruntergeladen am 17.11.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ijcre-2025-0010/pdf?lang=de
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