Near-Infrared Reflectance for Silica Surface Area Determination in Aerospace Materials

Authors

  • Amanda Inacio de Almeida Departamento de Ciência e Tecnologia Aeroespacial – Instituto Tecnológico de Aeronáutica – Divisão de Ciências Fundamentais – São José dos Campos/SP – Brazil. https://orcid.org/0009-0004-8029-0235
  • Rachel Farias de Margalhães Departamento de Ciência e Tecnologia Aeroespacial – Instituto Tecnológico de Aeronáutica – Divisão de Ciências Fundamentais – São José dos Campos/SP – Brazil. https://orcid.org/0000-0002-1364-3748
  • Milton Faria Diniz Departamento de Ciência e Tecnologia Aeroespacial – Instituto de Aeronáutica e Espaço – Divisão de Propulsão – São José dos Campos/SP – Brazil. https://orcid.org/0000-0003-0246-0660
  • Ademir de Oliveira Departamento de Ciência e Tecnologia Aeroespacial – Instituto de Aeronáutica e Espaço – Divisão de Propulsão – São José dos Campos/SP – Brazil. https://orcid.org/0000-0001-9884-2959
  • Javier Quagliano Instituto de Investigaciones Científicas y Técnicas para la Defensa – Applied Chemistry Department – Buenos Aires – Argentina. https://orcid.org/0000-0002-6549-983X
  • Natalia Sanches Centro de Tecnologia da Informação Renato Archer – Coordenação de Laboratórios Abertos e Parque Tecnológico – Campinas/SP – Brazil. https://orcid.org/0000-0002-3545-119X
  • Rita de Cássia Lazzarini Dutra Departamento de Ciência e Tecnologia Aeroespacial – Instituto Tecnológico de Aeronáutica – Divisão de Ciências Fundamentais – São José dos Campos/SP – Brazil. https://orcid.org/0000-0001-9958-1279

DOI:

https://doi.org/10.1590/jatm.v18.1452

Keywords:

Near infrared, Reflectance, Specific surface area, Silicon dioxide

Abstract

The specific surface area of a filler influences its dispersion and interaction with the rubber and consequently the properties of thermal insulation in aerospace components. However, its determination generally requires complex instrumental methods. Therefore, the development of simpler methodologies with equivalent or higher precision remains of scientific interest. This study investigates the application of Fourier transform infrared spectroscopy using near-infrared (NIR) reflectance and the more conventional diffuse reflectance for silica analysis, a filler widely used in polymeric formulations. The analyzed samples presented surface area values between 170 and 800 m2·g-1. Results showed a methodological error within the instrumental limit (2%), lower than that reported for conventional methods (4-7%). The NIR reflectance methodology based on the relative band (A5260/A4540) provided the most accurate results and can be considered a practical alternative to conventional gas adsorption techniques, enabling shorter analysis times, a feature that is particularly relevant for aerospace processes subject to demanding project schedules.


References

Acevedo NIA, Rocha MCG, Bertolino LC (2021) Determinação da área superficial específica e da porosidade de duas amostras de argilas provenientes da bacia de Taubaté - São Paulo. Braz Appl Sci Rev 5 (1):39-57. https://doi.org/10.34115/basrv5n1-004

Bar G, Amar L, Marszewski M, Bolker A, Dashti A, Dror R, Pilon L (2023) Synthesis of silica aerogel films in liquid molds. J Colloid Interface Sci 648:418-426. https://doi.org/10.1016/j.jcis.2023.06.004

Barros AH, Magalhães RF, Murakami LMS, Diniz MF, Sanches NB, Carvalho TA, Dutra JCN, Dutra RCL (2025) Determination of elastomer content in NR/SBR/BR blends. Polimeros 35(2):e20250023. https://doi.org/10.1590/0104-1428.20240110

Carvalho TA, Barros AH, Magalhães RF, Diniz MF, Murakami LMS, Dutra JCN, Sanches NB, Dutra RCL (2025) Quantification of elastomers in CR/NR/BR blends. Polimeros 35(3):e20250026. https://doi.org/10.1590/0104-1428.20240130

Chen Y, Lin M, Cai L (2025) Measurement of specific surface area of silica gel using a paper-based microscale laboratory. J Chem Educ 102:957-961. https://doi.org/10.1021/acs.jchemed.4c01355

Christy AA (2008) Quantitative determination of surface area of silica gel particles by near-infrared spectroscopy and chemometrics. Colloids Surf A Physicochem Eng Asp 322:248-252. https://doi.org/10.1016/j.colsurfa.2008.03.021

Domínguez JMA, Ramaye Y, Dabrio M, Kestens V (2020) Validation of a homogeneous incremental centrifugal liquid sedimentation method for size analysis of silica (nano)particles. Materials (Basel) 13 (17):3806. https://doi.org/10.3390/ma13173806

Elashker A, Zaghloul B, Eldakhakhny AM, Gobara M, Mokhtar M (2024) Study of thermal protection materials in solid propellant rocket engines. ASAT J 20:202403. [accessed Mar 15 2025]. https://www.researchgate.net/publication/378862930_Study_of_thermal_protection_materials_in_solid_propellant_rocket_engines

Ferraresi TM, Silva WTL, Martin-Neto L, Silveira PM, Madari BE (2012) Espectroscopia de infravermelho na determinação da textura do solo. Rev Bras Cienc Solo 36:1769-1777. https://doi.org/10.1590/S0100-06832012000600010

Fiedler R, Beizinger B, Walther P, Lindén M (2022) Synthesis of highly monodisperse superparamagnetic iron oxide core@ mesoporous silica shell particles with independently tunable size and porosity. Microporous Mesoporous Mater 340:112027. https://doi.org/10.1016/j.micromeso.2022.112027

Goddu RF (1960) Near-infrared spectrophotometry. Adv Anal Chem Instr 1:347-424.

Gómez-Tena MP, Gilabert J, Toledo J, Zumaqueri E, Machi C (2014) Relationship between the specific surface area parameters determined using different analytical techniques. Paper presented 2014 XII Foro Global del Recubrimiento Cerámico. Cámara Oficial de Comercio, Industria y Navegación de Castellón; Castellón, Spain. [accessed Mar 10 2025]. https://www.qualicer.org/recopilatorio/ponencias/pdfs/56%20POSTER%20ING.pdf

Harris S (2025) Thermal protection systems for reusable spacecraft: materials and performance. Am J Aerosp Aeronaut Eng 6(1):6-10. [accessed Aug 20 2025]. https://australiansciencejournals.com/ajaae

Horák MA, Vítek A (1978) Interpretation and processing of vibrational spectra. New York: Wiley.

Kestens V, Roebben G, Herrmann J, Jämting Å, Coleman V, Minelli C, Clifford C, De Temmerman PJ, Mast J, Liu JJ (2016) Challenges in the size analysis of a silica nanoparticle mixture as candidate certified reference material. J Nanopart Res 18(6):161. https://doi.org/10.1007/s11051-016-3474-2

Magalhães RF (2023) Avaliação de técnicas FT-IR de transmissão, reflexão e refletância para a caracterização/quantificação de polímeros e carga de diferentes setores industriais [doctoral dissertation]. São José dos Campos: Instituto Tecnológico de Aeronáutica. In Portuguese.

Magalhães RF, Barros AH, Takematsu MM, Passero A, Diniz MF, Sciamareli J, Dutra RCL (2022) Infrared reflectance techniques applied to silica particle diameter determination: theoretical and experimental data. An Acad Bras Cienc 94:e20210545. [accessed Mar 05 2025]. https://pubmed.ncbi.nlm.nih.gov/36259823/

McCool B, Murphy L, Tripp CP (2006) A simple FTIR technique for estimating the surface area of silica powders and films. J Colloid Interface Sci 295:294-298. https://doi.org/10.1016/j.jcis.2005.08.010

Moretto E, Stoffels C, Federico CE, Rogé V, Staropoli M, Imiete IE, Audinot JN, Steiner P, Duez B, Lenoble D, et al. (2023) Interplay of regio-selectively modified dendritic silica particles with styrene-butadiene rubber: the route towards better tires with lower rolling resistance and higher grip. Chem Eng J 461:141964. https://doi.org/10.1016/j.cej.2023.141964

Okoli U, Rishi K, Beaucage G, Kammler HK, McGlasson A, Chauby M, Kuppa VK (2023) Dispersion of modified fumed silica in elastomeric nanocomposites. Polymer (Guildf) 264:125407. https://doi.org/10.1016/j.polymer.2022.125407

Osswald J, Fehr KT (2006) FTIR spectroscopic study on liquid silica solutions and nanoscale particle size determination. J Mater Sci 41(5):1335-1339. https://doi.org/10.1007/s10853-006-7327-8

Padmanathan HR, Federico CE, Addiego F, Rommel R, Kotecký O, Westermann S, Fleming Y (2021) Influence of silica specific surface area on the viscoelastic and fatigue behaviors of silica-filled SBR composites. Polymers 13:3094. https://doi.org/10.3390/polym13183094

Pavia DL, Lampman GM, Kriz GS (2015) Introduction to spectroscopy. 5th ed. Stamford: Cengage Learning. [accessed Jan 10 2025]. https://dl.iranchembook.ir/ebook/organic-chemistry-2753.pdf

Ramos DM, Sadtler V, Marchal P, Lemaitre C, Benyahia L, Roques-Carmes T (2023) Properties of non-conventional direct O/W Pickering emulsions stabilized by partially hydrophobic silica particles controlled by rotor-stator or ultrasonic emulsification. Colloids Surf A Physicochem Eng Asp 673:131782. https://doi.org/10.1016/j.colsurfa.2023.131782

Schadosin J, Saab SC, Brinatti AM, Pires LF (2023) Quantitative and qualitative characterization of the granulometry of an Inceptisol. Quim Nova 46:329-335. https://doi.org/10.21577/0100-4042.20230018

Sharma J, Polizos G (2020) Hollow silica particles: recent progress and future perspectives. Nanomaterials (Basel) 10(8):1599. https://doi.org/10.3390/nano10081599

Silverstein RM, Webster FX, Kiemle DJ (2005) Spectrometric identification of organic compounds. 7th ed. Hoboken: John Wiley & Sons. [accessed Feb 15 2025]. https://eclass.upatras.gr/modules/document/file.php/PHY1973/Silverstein%20-%20

Smith AL, editor (1979) Applied infrared spectroscopy: fundamentals, techniques and analytical problem-solving. New York: John Wiley & Sons.

Sowinska-Baranowska A, Maciejewska M (2021) Influence of the silica specific surface area and ionic liquids on the curing characteristics and performance of styrene-butadiene rubber. Materials 14:5302. https://doi.org/10.3390/ma14185302

Stach R, Barone T, Cauda E, Krebs P, Pejcic B, Daboss S, Mizaikoff B (2020) Direct infrared spectroscopy for size-independent identification and quantification of respirable particles relative mass in mine dusts. Anal Bioanal Chem 412(14):3499-3508. https://doi.org/10.1007/s00216-020-02565-0

Thommes M, Kaneko K, Neimark AV, Olivier JP, Rodriguez-Reinoso F, Rouquerol J, Sing KSW (2015) Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report). Pure Appl Chem 87(9-10):1051-1069. https://doi.org/10.1515/pac-2014-1117

Uniyal P, Gaur P, Yadav J, Bhalla NA, Khan T, Junaedi H, Sebaey TA (2025) A comprehensive review on the role of nanosilica as a toughening agent for enhanced epoxy composites for aerospace applications. ACS Omega 10:15810-15839. https://doi.org/10.1021/acsomega.4c10073

Yassin FM, Fathy MM, Fahmy HM, Elshemy WM (2021) Low-angle X-ray scattering for determining the size of mesoporous silica nanoparticles. Radiat Phys Chem 179:109235. https://doi.org/10.1016/j.radphyschem.2020.109235

Downloads

Published

2026-08-10

Issue

Vol. 18 (2026)

Section

Original Paper

License

Copyright (c) 2026 Amanda Inacio de Almeida, Rachel Farias de Margalhães, Milton Faria Diniz, Ademir de Oliveira, Javier Quagliano, Natalia Sanches, Rita de Cássia Lazzarini Dutra

Creative Commons License

This work is licensed under a Creative Commons Attribution 4.0 International License.

This work is licensed under a Creative Commons — Attribution 4.0 International — CC BY 4.0. Authors are free to Share (copy and redistribute the material in any medium or format) and Adapt (remix, transform, and build upon the material for any purpose, even commercially). JATM allow the authors to retain publishing rights without restrictions.