Araştırma Makalesi
BibTex RIS Kaynak Göster

TG-DTG/DSC, XRD, SEM VE FTIR ANALİZLERİ KULLANILARAK YÜKSEK SICAKLIK KOŞULLARINA MARUZ KALAN ÇİMENTO HAMURUNUN BOZULMASININ KARAKTERİZASYONU

Yıl 2026, Cilt: 46 Sayı: 1 , 130 - 140 , 01.05.2026
https://doi.org/10.47480/isibted.1800582
https://izlik.org/JA37AA77PS

Öz

CEM I çimento hamurunun yüksek sıcaklık davranışı, 25 ila 1000°C arasında hava atmosferinde meydana gelen yapısal ve kimyasal değişiklikleri değerlendirmek için TG–DTG/DSC, BET, XRD, SEM ve FTIR analizleri kullanılarak incelenmiştir. TG–DTG/DSC deneylerinden elde edilen bozunma profilleri üç farklı bölge ortaya koymuştur: (i) C–S–H jelinin ve gözenek suyunun dehidratasyonu, (ii) portlanditin dehidroksilasyonu ve (iii) kalsitin dekarbonasyonu. Her bozunma adımı için karakteristik sıcaklıklar belirlenmiş ve kinetik parametreler Ortega yöntemi kullanılarak hesaplanmıştır. BET analizi, mikro gözenekli yapının kapsamlı bir şekilde çatladığını gösterirken, XRD, SEM ve FTIR, yüksek sıcaklıklara maruz kalan çimento hamurlarındaki faz dönüşümleri ve mikro yapısal evrim hakkında bilgi sağlamıştır. Isıtma hızının (2,5, 10 ve 20°C·dak-1) termal davranış üzerindeki etkisi de değerlendirilmiş ve bozunma süreçleri üzerindeki etkisi vurgulanmıştır. Bu bulgular, çimentolu malzemelerin yangın koşullarındaki termal kararlılığı ve bozunma mekanizmalarının daha iyi anlaşılmasına katkıda bulunmaktadır.

Destekleyen Kurum

ATATÜRK ÜNİVERSİTESİ BAP KOORDİNATÖRLÜĞÜ

Proje Numarası

FHD-2018-6654

Kaynakça

  • Abdelmelek, N., Lubloy, E. (2021). Evaluation of the mechanical properties of high strength cement paste at elevated temperatures using metakaolin. Journal of Thermal Analysis and Calorimetry, 145, 2891–2905. https://doi.org/10.1007/s10973-020-09992-2
  • Alarcon-Ruiz, L., Platret, G., Massieu, E., Ehrlacher, A. (2005). The use of thermal analysis in assessing the effect of temperature on a cement paste. Cement and Concrete Research, 35(3), 609–613. https://doi.org/10.1016/j.cemconres.2004.06.015
  • Alanso, M.M., Palacios, M., Puertas, F. (2013). Effect of polycarboxylate-ether admixtures on calcium aluminate cement pastes, Part 2: Hydration studies. Industrial & Engineering Chemistry Research, 52, 17330-17340. https://doi.org/10.1021/ie401616f
  • Arıöz, Ö. (2007). Effects of elevated temperatures on properties of concrete. Fire Safety Journal, 42(8), 516–522. https://doi.org/10.1016/j.firesaf.2007.01.003
  • Bakharev, T. (2005). Geopolymeric materials prepared using class F fly ash and elevated temperature curing. Cement and Concrete Research, 35(6), 1224. https://doi.org/10.1016/j.cemconres.2004.06.031
  • Bingöl, A.F., Gül, R. (2004). Compressive strength of lightweight aggregate concrete exposed to high temperatures. Indian Journal of Engineering and Materials Sciences, 11, 68–72.
  • Bingöl, A.F., Gül, R. (2009). Effect of elevated temperatures and cooling regimes on normal strength concrete. Fire and Materials, 33, 79–88. https://doi.org/10.1002/fam.987
  • Boquera, L., Castro, J.R., Pisello, A.L., Fabiani, C., D’Alessandro, A., Ubertini, F., Cabeza, L.F. (2021). Thermal and mechanical performance of cement paste under high temperature thermal cycles. Solar Energy Materials and Solar Cells, 231, 111333. https://doi.org/10.1016/j.solmat.2021.111333
  • European Committee for Standardization. (2000). Cement: Common cements (PrEN 197-1, CEN/TC51/WG 6 rev., Final Draft).
  • Gadsden, J.A. (1975). Infrared spectra of minerals and related inorganic compounds (3rd ed.). Butterworths. Handoo, S.K., Agarwal, S., Agarwal, S.K. (2002). Physicochemical, mineralogical, and morphological characteristics of concrete exposed to elevated temperatures. Cement and Concrete Research, 32, 1009–1018. https://doi.org/10.1016/S0008-8846(01)00736-0
  • Hüsem, M. (2006). The effects of high temperature on compressive and flexural strengths of ordinary and high- performance concrete. Fire Safety Journal, 41, 155–163. https://doi.org/10.1016/j.firesaf.2005.12.002
  • Kasaniya, M., Thomas, M.D.A., Moffatt, T., Hossack, A. (2024). Microstructure and microanalysis of Portland cement pastes with high w/c ratios. Cement and Concrete Research, 183, 107575. https://doi.org/10.1016/j.cemconres.2024.107575
  • Khoury, G.A. (1992). Compressive strength of concrete at high temperatures: Reassessment. Magazine of Concrete Research, 44, 291–309. https://doi.org/10.1680/macr.1992.44.161.291
  • Kontori, E., Perraki, T., Tsivilis, S., Kakali, G. (2009). Zeolite blended cements: Evaluation of their hydration rate by means of thermal analysis. Journal of Thermal Analysis and Calorimetry, 96, 993–998. http://doi.org/10.1007/s10973-009-0056-x
  • Li, S., Whitely, N., Xu, W., Pan, W.P. (2005). Characterization of Coal by Thermal Analysis Methods, Thermal Analysis Laboratory, Materials Characterization Centre, Western Kentucky University.
  • Li, Y., Luo, Y., Du, H., Liu, W., Tang, L., Xing, F. (2022). Evolution of microstructural characteristics of carbonated cement pastes subjected to high temperatures evaluated by MIP and SEM. Materials, 15, 6037. https://doi.org/10.3390/ma15176037
  • Matossi, F. (1949). Vibration frequencies and binding forces in some silicate groups. Journal of Chemical Physics, 17, 679. https://doi.org/10.1063/1.1747369
  • Odler, I. (2003). The BET-specific surface area of hydrated Portland cement and related materials. Cement and Concrete Research, 33, 2049–2056. https://doi.org/10.1016/S0008-8846(03)00225-4
  • Ortega, A. (1996). Some successes and failures of the methods based on several experiments. Thermochimica Acta, 284, 379–387. https://doi.org/10.1016/0040-6031(95)02766-1
  • Peng, G.F., Huang, Z.S. (2008). Change in microstructure of hardened cement paste subjected to elevated temperatures. Construction and Building Materials, 22, 593. https://doi.org/10.1016/j.conbuildmat.2006.11.002
  • Poon, C.S., Azhar, S., Anson, M., Wong, Y.L. (2001). Comparison of the strength and durability performance of normal and high- strength pozzolanic concretes at elevated temperatures. Cement and Concrete Research, 31(9), 1291–1300. https://doi.org/10.1016/S0008-8846(01)00580-4
  • Poon, C.S., Azhar, S., Anson, M., Wong, Y.L. (2003). Performance of metakaolin concrete at elevated temperatures. Cement and Concrete Composites, 25(1), 83–89. https://doi.org/10.1016/S0958-9465(01)00061-0
  • Poon, C.S., Shui, Z. H., Lam, L. (2004). Compressive behavior of fiber reinforced high-performance concrete subjected to elevated temperatures. Cement and Concrete Research, 34, 2215–2222. https://doi.org/10.1016/j.cemconres.2004.02.011
  • Tantawy, M.A. (2017). Effect of high temperatures on the microstructure of cement paste. Journal of Materials Science and Chemical Engineering, 5, 33–48. http://doi.org/10.4236/msce.2017.511004
  • Thomas, J.J., Jennings, H.M., Allen, A.J. (1999). The surface area of hardened cement paste as measured by various techniques. Concrete Science and Engineering, 1, 45–64. https://doi.org/10.1016/S0008-8846(98)00049-0
  • TS EN 12390-3. (2010). Beton-Sertleşmiş beton deneyleri- Bölüm 3: Deney numunelerinin basınç dayanımının tayini, Türk Standartları Enstitüsü, Ankara, Türkiye.
  • Zhang, Q., Ye, G. (2011). Microstructure analysis of heated Portland cement paste. Procedia Engineering, 14, 830–836. https://doi.org/10.1016/j.proeng.2011.07.105
  • Zhang, Q., Ye, G. (2012). Dehydration kinetics of Portland cement paste at high temperature. Journal of Thermal Analysis and Calorimetry, 110, 153–158. http://doi.org/10.1007/s10973-012-2303-9

A CHARACTERIZATION OF CEMENT PASTE DEGRADATION EXPOSED TO ELEVATED TEMPERATURES CONDITIONS USING TG-DTG/DSC, XRD, SEM, AND FTIR ANALYSES

Yıl 2026, Cilt: 46 Sayı: 1 , 130 - 140 , 01.05.2026
https://doi.org/10.47480/isibted.1800582
https://izlik.org/JA37AA77PS

Öz

The high-temperature behavior of CEM I cement paste was investigated using TG–DTG/DSC, BET, XRD, SEM, and FTIR analyses to evaluate the structural and chemical modifications occurring between 25 and 1000°C under air atmosphere. The degradation profiles from TG–DTG/DSC experiments revealed three distinct regions: (i) dehydration of the C–S–H gel and pore water, (ii) dehydroxylation of portlandite, and (iii) decarbonation of calcite. Characteristic temperatures for each degradation step were determined, and kinetic parameters were calculated using the Ortega method. BET analysis indicated extensive cracking of the micropore structure, while XRD, SEM, and FTIR provided insights into phase transformations and microstructural evolution in cement pastes exposed to elevated temperatures. The effect of heating rate (2.5, 10, and 20°C·min-1) on thermal behavior was also assessed, highlighting its influence on the degradation processes. These findings contribute to a better understanding of the thermal stability and degradation mechanisms of cementitious materials under fire conditions.

Proje Numarası

FHD-2018-6654

Kaynakça

  • Abdelmelek, N., Lubloy, E. (2021). Evaluation of the mechanical properties of high strength cement paste at elevated temperatures using metakaolin. Journal of Thermal Analysis and Calorimetry, 145, 2891–2905. https://doi.org/10.1007/s10973-020-09992-2
  • Alarcon-Ruiz, L., Platret, G., Massieu, E., Ehrlacher, A. (2005). The use of thermal analysis in assessing the effect of temperature on a cement paste. Cement and Concrete Research, 35(3), 609–613. https://doi.org/10.1016/j.cemconres.2004.06.015
  • Alanso, M.M., Palacios, M., Puertas, F. (2013). Effect of polycarboxylate-ether admixtures on calcium aluminate cement pastes, Part 2: Hydration studies. Industrial & Engineering Chemistry Research, 52, 17330-17340. https://doi.org/10.1021/ie401616f
  • Arıöz, Ö. (2007). Effects of elevated temperatures on properties of concrete. Fire Safety Journal, 42(8), 516–522. https://doi.org/10.1016/j.firesaf.2007.01.003
  • Bakharev, T. (2005). Geopolymeric materials prepared using class F fly ash and elevated temperature curing. Cement and Concrete Research, 35(6), 1224. https://doi.org/10.1016/j.cemconres.2004.06.031
  • Bingöl, A.F., Gül, R. (2004). Compressive strength of lightweight aggregate concrete exposed to high temperatures. Indian Journal of Engineering and Materials Sciences, 11, 68–72.
  • Bingöl, A.F., Gül, R. (2009). Effect of elevated temperatures and cooling regimes on normal strength concrete. Fire and Materials, 33, 79–88. https://doi.org/10.1002/fam.987
  • Boquera, L., Castro, J.R., Pisello, A.L., Fabiani, C., D’Alessandro, A., Ubertini, F., Cabeza, L.F. (2021). Thermal and mechanical performance of cement paste under high temperature thermal cycles. Solar Energy Materials and Solar Cells, 231, 111333. https://doi.org/10.1016/j.solmat.2021.111333
  • European Committee for Standardization. (2000). Cement: Common cements (PrEN 197-1, CEN/TC51/WG 6 rev., Final Draft).
  • Gadsden, J.A. (1975). Infrared spectra of minerals and related inorganic compounds (3rd ed.). Butterworths. Handoo, S.K., Agarwal, S., Agarwal, S.K. (2002). Physicochemical, mineralogical, and morphological characteristics of concrete exposed to elevated temperatures. Cement and Concrete Research, 32, 1009–1018. https://doi.org/10.1016/S0008-8846(01)00736-0
  • Hüsem, M. (2006). The effects of high temperature on compressive and flexural strengths of ordinary and high- performance concrete. Fire Safety Journal, 41, 155–163. https://doi.org/10.1016/j.firesaf.2005.12.002
  • Kasaniya, M., Thomas, M.D.A., Moffatt, T., Hossack, A. (2024). Microstructure and microanalysis of Portland cement pastes with high w/c ratios. Cement and Concrete Research, 183, 107575. https://doi.org/10.1016/j.cemconres.2024.107575
  • Khoury, G.A. (1992). Compressive strength of concrete at high temperatures: Reassessment. Magazine of Concrete Research, 44, 291–309. https://doi.org/10.1680/macr.1992.44.161.291
  • Kontori, E., Perraki, T., Tsivilis, S., Kakali, G. (2009). Zeolite blended cements: Evaluation of their hydration rate by means of thermal analysis. Journal of Thermal Analysis and Calorimetry, 96, 993–998. http://doi.org/10.1007/s10973-009-0056-x
  • Li, S., Whitely, N., Xu, W., Pan, W.P. (2005). Characterization of Coal by Thermal Analysis Methods, Thermal Analysis Laboratory, Materials Characterization Centre, Western Kentucky University.
  • Li, Y., Luo, Y., Du, H., Liu, W., Tang, L., Xing, F. (2022). Evolution of microstructural characteristics of carbonated cement pastes subjected to high temperatures evaluated by MIP and SEM. Materials, 15, 6037. https://doi.org/10.3390/ma15176037
  • Matossi, F. (1949). Vibration frequencies and binding forces in some silicate groups. Journal of Chemical Physics, 17, 679. https://doi.org/10.1063/1.1747369
  • Odler, I. (2003). The BET-specific surface area of hydrated Portland cement and related materials. Cement and Concrete Research, 33, 2049–2056. https://doi.org/10.1016/S0008-8846(03)00225-4
  • Ortega, A. (1996). Some successes and failures of the methods based on several experiments. Thermochimica Acta, 284, 379–387. https://doi.org/10.1016/0040-6031(95)02766-1
  • Peng, G.F., Huang, Z.S. (2008). Change in microstructure of hardened cement paste subjected to elevated temperatures. Construction and Building Materials, 22, 593. https://doi.org/10.1016/j.conbuildmat.2006.11.002
  • Poon, C.S., Azhar, S., Anson, M., Wong, Y.L. (2001). Comparison of the strength and durability performance of normal and high- strength pozzolanic concretes at elevated temperatures. Cement and Concrete Research, 31(9), 1291–1300. https://doi.org/10.1016/S0008-8846(01)00580-4
  • Poon, C.S., Azhar, S., Anson, M., Wong, Y.L. (2003). Performance of metakaolin concrete at elevated temperatures. Cement and Concrete Composites, 25(1), 83–89. https://doi.org/10.1016/S0958-9465(01)00061-0
  • Poon, C.S., Shui, Z. H., Lam, L. (2004). Compressive behavior of fiber reinforced high-performance concrete subjected to elevated temperatures. Cement and Concrete Research, 34, 2215–2222. https://doi.org/10.1016/j.cemconres.2004.02.011
  • Tantawy, M.A. (2017). Effect of high temperatures on the microstructure of cement paste. Journal of Materials Science and Chemical Engineering, 5, 33–48. http://doi.org/10.4236/msce.2017.511004
  • Thomas, J.J., Jennings, H.M., Allen, A.J. (1999). The surface area of hardened cement paste as measured by various techniques. Concrete Science and Engineering, 1, 45–64. https://doi.org/10.1016/S0008-8846(98)00049-0
  • TS EN 12390-3. (2010). Beton-Sertleşmiş beton deneyleri- Bölüm 3: Deney numunelerinin basınç dayanımının tayini, Türk Standartları Enstitüsü, Ankara, Türkiye.
  • Zhang, Q., Ye, G. (2011). Microstructure analysis of heated Portland cement paste. Procedia Engineering, 14, 830–836. https://doi.org/10.1016/j.proeng.2011.07.105
  • Zhang, Q., Ye, G. (2012). Dehydration kinetics of Portland cement paste at high temperature. Journal of Thermal Analysis and Calorimetry, 110, 153–158. http://doi.org/10.1007/s10973-012-2303-9
Toplam 28 adet kaynakça vardır.

Ayrıntılar

Birincil Dil İngilizce
Konular Kimya Mühendisliği (Diğer)
Bölüm Araştırma Makalesi
Yazarlar

Jale Naktiyok 0000-0002-6316-4112

Duygu Adigüzel 0000-0002-8854-5501

Ahmet Ferhat Bingöl 0000-0002-8798-8343

Proje Numarası FHD-2018-6654
Gönderilme Tarihi 10 Ekim 2025
Kabul Tarihi 18 Şubat 2026
Yayımlanma Tarihi 1 Mayıs 2026
DOI https://doi.org/10.47480/isibted.1800582
IZ https://izlik.org/JA37AA77PS
Yayımlandığı Sayı Yıl 2026 Cilt: 46 Sayı: 1

Kaynak Göster

APA Naktiyok, J., Adigüzel, D., & Bingöl, A. F. (2026). A CHARACTERIZATION OF CEMENT PASTE DEGRADATION EXPOSED TO ELEVATED TEMPERATURES CONDITIONS USING TG-DTG/DSC, XRD, SEM, AND FTIR ANALYSES. Isı Bilimi ve Tekniği Dergisi, 46(1), 130-140. https://doi.org/10.47480/isibted.1800582