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Journals / Gazi Üniversitesi Mühendislik Mimarlık Fakültesi Dergisi / 2026 / Cilt: 41 Sayı: 2

Investigation of thermal oxidative stabilization process of viscose rayon fibers by multi-step heat treatment technique

Çok adımlı ısıl işlem tekniğiyle viskoz rayon liflerin termal oksidatif stabilizasyon sürecinin incelenmesi

Tuba Demirel(HASAN KALYONCU ÜNİVERSİTESİ, MÜHENDİSLİK FAKÜLTESİ, MAKİNE MÜHENDİSLİĞİ BÖLÜMÜ)0000-0002-5760-3705
Kemal Şahin Tunçel(SİİRT ÜNİVERSİTESİ)0000-0001-5095-6543
İsmail Karacan(ERCİYES ÜNİVERSİTESİ, MÜHENDİSLİK FAKÜLTESİ)0000-0002-9047-1011
Pages
1091–1102
Publication Date
2026-07-20
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AI Summary & Key Takeaways

AI Insight
⚡ TL;DR(Too Long; Didn't Read)

The results show that as the TOS time increased, the density increased to 1.73 g/cm3 and the carbonization efficiency increased from 15% to 64%, but the tensile strength decreased by 60%.

📌 3 Key Takeaways

🎯
Objective & Hypothesis:This study investigates the thermal oxidative stabilization (TOS) process of viscose rayon fibers.
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Key Findings & Data:Before stabilization, a chemical pretreatment containing ammonium sulfamate and urea was applied to the fibers, and then stabilization was carried out at temperatures between 200 °C - 250 °C for different times with a multi-step heat treatment strategy.
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Conclusion & Impact:The results show that as the TOS time increased, the density increased to 1.73 g/cm3 and the carbonization efficiency increased from 15% to 64%, but the tensile strength decreased by 60%.
🔬Design:Modeling & Simulation
📍Scope:Comprehensive Sample
⚙️Variables:Viskoz rayon · aktif karbon · amonyum sülfamat

Abstract

This study investigates the thermal oxidative stabilization (TOS) process of viscose rayon fibers. Before stabilization, a chemical pretreatment containing ammonium sulfamate and urea was applied to the fibers, and then stabilization was carried out at temperatures between 200 °C - 250 °C for different times with a multi-step heat treatment strategy. The effects of the TOS process on fiber density, tensile strength, FT-IR spectroscopy, X-ray diffraction (XRD), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were evaluated in detail. The results show that as the TOS time increased, the density increased to 1.73 g/cm3 and the carbonization efficiency increased from 15% to 64%, but the tensile strength decreased by 60%. FT-IR and XRD analyses revealed that the cellulose II crystal structure was disrupted, the structure became 100% amorphous after 5 min of stabilization and cross-linked aromatic structures increased. DSC and TGA results show that the thermal resistance of stabilized fibers is significantly improved. These findings indicate that stabilized viscose rayon fibers have attained sufficient thermal stability for the subsequent stages while also making significant contributions to the optimization processes for the efficient production of viscose rayon-based activated carbon fibers.

Özet

Bu çalışma, viskoz rayon liflerin termal oksidatif stabilizasyon (TOS) sürecini incelemektedir. Stabilizasyon öncesinde liflere amonyum sülfamat ve üre içeren bir kimyasal ön işlem uygulanmış, ardından çok adımlı bir ısıl işlem stratejisi ile 200°C-250°C arasındaki sıcaklıklarda farklı sürelerde stabilizasyon gerçekleştirilmiştir. TOS sürecinin lif yoğunluğu, mukavemet, FT-IR spektroskopisi, X-ışını kırınımı (XRD), diferansiyel taramalı kalorimetri (DSC) ve termogravimetrik analiz (TGA) üzerindeki etkileri detaylı olarak değerlendirilmiştir. Sonuçlar, TOS süresi arttıkça yoğunluğun 1,73 g/cm3 değerine ve kömürleşme veriminin %15’den %64’e yükseldiğini, ancak gerilme mukavemetinin ise %60 oranında azaldığını göstermektedir. FT-IR ve XRD analizleri, selüloz II kristal yapısının bozulduğunu, 5 dakikalık stabilizasyon sonrasında yapının %100 amorflaştığını ve çapraz bağlı aromatik yapıların arttığını ortaya koymuştur. DSC ve TGA sonuçları ise, stabilize edilmiş liflerin termal dayanıklılığının önemli ölçüde iyileştiğini göstermektedir. Bu bulgular, stabilize olmuş viskoz rayon liflerin sonraki aşamalar için yeterli termal kararlılığa ulaştığını gösterirken diğer yandan viskoz rayon esaslı aktif karbon liflerinin verimli bir şekilde üretimi için optimizasyon süreçlerine önemli katkılar sağlamaktadır.

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Cite This Article

Demirel, T., Tunçel, K. Ş., Karacan, İ. (2026). Investigation of thermal oxidative stabilization process of viscose rayon fibers by multi-step heat treatment technique. Gazi Üniversitesi Mühendislik Mimarlık Fakültesi Dergisi, Cilt: 41 Sayı: 2, 1091–1102. https://doi.org/10.17341/gazimmfd.1696408

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References (40)

  1. Ghahramani, P., Eldyasti, A., Leung, S.N., Open-cell polyvinylidene fluoride foams as carriers to promote biofilm growth for biological wastewater treatment. Polymer Engineering & Science, 61 (8), 2161–2171, 2021.
  2. Ayranci, E. Hoda, N., Adsorption kinetics and isotherms of pesticides onto activated carbon-cloth. Chemosphere, 60 (11), 1600–1607, 2005.
  3. Gupta, V.K. Suhas, Application of low-cost adsorbents for dye removal -A review. Journal Of Environmental Management, 90 (8), 2313–2342, 2009.
  4. Hina, K., Zou, H., Qian, W., Zuo, D., Yi, C., Preparation and performance comparison of cellulose-based activated carbon fibres. Cellulose, 25 (1), 607–617, 2018.
  5. Sun, J., Wu, L., Wang, Q., Comparison about the structure and properties of PAN-based activated carbon hollow fibers pretreated with different compounds containing phosphorus. Journal Of Applied Polymer Science, 96 (2), 294–300, 2005.
  6. Gül A., Investigation of the structural transformations of phosphoric acid impregnated viscose rayon fibers during the thermal stabilization stage before carbonization, Journal of the Faculty of Engineering and Architecture of Gazi University, 40 (2), 749–760, 2025.
  7. Guo, Y. Rockstraw, D.A., Physical and chemical properties of carbons synthesized from xylan, cellulose, and Kraft lignin by H3PO4 activation. Carbon, 44 (8), 1464–1475, 2006.
  8. Zeng, F., Pan, D., Pan, N., Choosing the impregnants by thermogravimetric analysis for preparing rayon-based carbon fibers. Journal Of Inorganic And Organometallic Polymers And Materials, 15 (2), 261–267, 2005.
  9. Zeng, F. Pan, D., The structural transitions of rayon under the promotion of a phosphate in the preparation of ACF. Cellulose, 15 (1), 91–99, 2008.
  10. Su, C.-I. Wang, C.-L., Optimum manufacturing conditions of activated carbon fiber absorbents. I. Effect of flame retardant reagent concentration. Fibers and Polymers, 8 (5), 477–481, 2007.
  11. You, S. Y., Park, Y. H., Park, C. R., Preparation and properties of activated carbon fabric from acrylic fabric waste. Carbon, 38 (10), 1453–1460, 2000.
  12. Worasuwannarak, N., Hatori, S., Nakagawa, H., Miura, K., Effect of oxidation pre-treatment at 220 to 270°C on the carbonization and activation behavior of phenolic resin fiber. Carbon, 41 (5), 933–944, 2003.
  13. Fu, R., Liu, L., Huang, W., Sun, P., Studies on the structure of activated carbon fibers activated by phosphoric acid. Journal of Applied Polymer Science, 87 (14), 2253–2261, 2003.
  14. Rosas, J. M., Bedia, J., Rodríguez-Mirasol, J., Cordero, T., Hemp-derived activated carbon fibers by chemical activation with phosphoric acid. Fuel, 88 (1), 19–26, 2009.
  15. Williams, P. T. Reed, A. R., High grade activated carbon matting derived from the chemical activation and pyrolysis of natural fibre textile waste. Journal of Analytical and Applied Pyrolysis, 71 (2), 971–986, 2004.
  16. Su, C.-I., Peng, C.-C., Lee, C.-Y., Performance of viscose rayon based activated carbon fabric modified by sputtering silver and continuous plasma treatment. Textile Research Journal, 81 (7), 730–737, 2011.
  17. Gül, A., A study on structural changes during the thermal stabilization stage of hemp fibers impregnated with phosphoric acid before carbonization and activation, Fibers and Polymers, 26 (16), 685-696, 2025.
  18. Hariri, H., Tunçel, K.Ş., Karacan, I., Structure and properties of thermally stabilized and ecologically friendly organic cotton fibers as a new activated carbon fiber precursor. Fibers and Polymers, 25 (8), 2925–2933, 2024.
  19. Tunçel, K.Ş., Fosforik asidin rejenere selüloz esaslı lifler üzerine etkisi. Mühendislik Bilimleri ve Tasarım Dergisi, 8 (2), 605–611, 2020.
  20. Mwaikambo, L.Y. Ansell, M. P., Chemical modification of hemp, sisal, jute, and kapok fibers by alkalization. Journal of Applied Polymer Science, 84 (12), 2222–2234, 2002.
  21. Karacan, I. Soy, T., Structure and properties of oxidatively stabilized viscose rayon fibers impregnated with boric acid and phosphoric acid prior to carbonization and activation steps. Journal of Materials Science, 48 (5), 2009–2021, 2013.
  22. Kondo, T., The assignment of IR absorption bands due to free hydroxyl groups in cellulose. Cellulose, 4 (4), 281–292, 1997.
  23. Oh, S. Y., Yoo, D. I., Shin, Y., Kim, H. C., Kim, H. Y., Chung, Y. S., Park, W. H., Youk, J. H., Crystalline structure analysis of cellulose treated with sodium hydroxide and carbon dioxide by means of X-ray diffraction and FTIR spectroscopy. Carbohydrate Research, 340 (15), 2376–2391, 2005.
  24. Dadashian, F., Yaghoobi, Z., Wilding, M. A., Thermal behaviour of lyocell fibres. Polymer Testing, 24 (8), 969–977, 2005.
  25. Rafidison, B. H., Ramasawmy, H., Chummun, J., Florens, F.B.V., Using infrared spectrum analyses to predict tensile strength of fibres in a group of closely related plant species: case of Mascarenes Pandanus spp. SN Applied Sciences, 2 (1), 1922, 2020.
  26. Nelson, M. L. O’Connor, R.T., Relation of certain infrared bands to cellulose crystallinity and crystal lattice type. Part II. A new infrared ratio for estimation of crystallinity in celluloses I and II. Journal of Applied Polymer Science, 8 (3), 1325–1341, 1964.
  27. O’Connor, R.T., DuPré, E.F., Mitcham, D., Applications of infrared absorption spectroscopy to investigations of cotton and modified cottons: Part I: Physical and crystalline modifications and oxidation. Textile Research Journal, 28 (5), 382–392, 1958.
  28. Puziy, A.M., Poddubnaya, O.I., Martínez-Alonso, A., Suárez-García, F., Tascón, J.M.D., Surface chemistry of phosphorus-containing carbons of lignocellulosic origin. Carbon, 43 (14), 2857–2868, 2005.
  29. Carrillo, F., Colom, X., Suñol, J. J., Saurina, J., Structural FTIR analysis and thermal characterisation of lyocell and viscose-type fibres. European Polymer Journal, 40 (9), 2229–2234, 2004.
  30. Gaan, S., Sun, G., Effect of phosphorus and nitrogen on flame retardant cellulose: A study of phosphorus compounds. Journal of Analytical and Appied Pyrolysis, 78 (2), 371-377, 2007.
  31. Tunçel, K.Ş., Kimyasal modifikasyon sonrası termal olarak stabilize edilen viskoz rayon liflerin yapısal analizi. KSÜ Mühendislik Bilimleri Dergisi, 28 (2), 823-834, 2025.
  32. Konstantopoulos, G., Soulis, S., Dragatogiannis, D., Charitidis, C., Introduction of a methodology to enhance the stabilization process of PAN fibers by modeling and advanced characterization. Materials, 13 (12), 2749-2775, 2020.
  33. Yusof, N., Rana, D., Ismail, A. F., Matsuura, T., Microstructure of polyacrylonitrile-based activated carbon fibers preparedfrom solvent-free coagulation process. Journal of Applied Research and Technology, 14 (1), 54-61, 2016.
  34. Yu, M.J., Bai, Y.J., Wang, C.G., Xu, Y., Guo, P.Z., A new method for the evaluation of stabilization index of polyacrylonitrile fibers. Materials Letters, 61 (11), 2292-2294, 2007.
  35. Di Dario, M.M., Stabilized-flameproofed fabric and method. US 2,771,379 1956.
  36. Kazachenko, A.S., Vasilieva, N.Y., Berezhnaya, Y.D., Fetisova, O.Y., Borovkova, V.S., Malyar, Y.N., Sudakova, I.G., Sychev, V.V., Issaoui, N., Lutoshkin, M.A., Karacharov, A.A., Sulfation of birch wood microcrystalline cellulose with sulfamic acid using ion-exchange resins as catalysts. Polymers, 15 (5), 1116-1130, 2023.
  37. Thomas, J.C., Process for the preparation of cellulose sulfate. US 2,511,229 1950.
  38. Hindeleh, A.H., Johnson, D.J., Montague, P.E., Fibre diffraction methods. In: French, A.D., Gardner, K.H., (eds) ACS Symposium No.141. American Chemical Society, Washington DC, pp 149-181, 1983.
  39. Bengtsson, A., Bengtsson, J., Sedin, M., Sjöholm, E., Carbon fibers from lignin-cellulose precursors: Effect of stabilization conditions. ACS Sustainable Chemistry & Engineering, 7 (9), 8440-8448, 2019.
  40. Rafidison, B. H., Ramasawmy, H., Chummun, J., Florens, F.B.V., Using infrared spectrum analyses to predict tensile strength of fibres in a group of closely related plant species: case of Mascarenes Pandanus spp. SN Applied Sciences, 2 (1), 1922, 2020.