Rheological and Structural Evaluation of Dental Flowable Composites for Optimized Performance in Transparent Aligner Systems
Abstract
1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Sample Preparation
2.3. Morphological and Compositional Characterization of Cured Resins
2.4. Thermogravimetric Analysis (TGA) on Cured Resins
2.5. UV-Vis and FT-IR Spectroscopy on Cured Resins
2.6. Rheological Characterization on Uncured and Cured Resins
2.7. Indentation Testing on Cured Resins
3. Results
3.1. Morphology and Elemental Analysis of the Cured Resin
3.2. Thermogravimetric Analysis (TGA and DTG) of the Cured Resin
3.3. Spectroscopic Characterization of the Cured Resin
3.4. Rheological Characterization
3.4.1. Viscosity of Uncured Resins
3.4.2. Viscoelastic Behavior Before and After Curing
3.5. Flat Indentation of the Cured Resin
4. Discussion
4.1. Microstructural and Compositional Implications for Orthodontic Attachments
4.2. Optical and Rheological Implications for Clinical Performance
5. Conclusions
- Post-curing mechanical properties varied significantly, with storage modulus spanning nearly two orders of magnitude (~0.06–5 MPa).
- Elastic modulus ranged from ~20 MPa to ~1000 MPa, highlighting substantial differences in stiffness among materials.
- SEM/EDX and TGA analyses showed overall consistency with manufacturer specifications, while revealing subtle variations in filler content and heterogeneous filler distribution.
- UV–Vis–NIR spectroscopy provided distinct spectral fingerprints, reflecting differences in filler composition and polymer matrix structure.
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Abbreviations
| Bis-EMA | Bisphenol A diglycidyl methacrylate ethoxylated |
| Bis-GMA | Bisphenol A-glycidyl methacrylate |
| CAD | Computer-aided design |
| CAM | Computer-aided manufacturing |
| CAT | Clear aligner therapy |
| DMA | Dimetacrylate |
| DTG | Derivative thermogravimetric |
| DUDMA | Diurethane dimethacrylate |
| EDX | Energy-Dispersive X-ray Spectroscopy |
| EGBADMA | Ethylene glycol bisphenol A dimethacrylate |
| EVA | Ethylene vinyl acetate |
| HEDMA | Hydroxyethyldimethacrylate |
| LVR | Linear viscoelastic region |
| SEM | Scanning electron microscopy |
| TEGDMA | Triethylene Glycol Dimethacrylate |
| TGA | Thermogravimetric analyses |
| UDMA | Urethane dimethacrylate |
References
- Palmieri, E.; Montaina, L.; Bellisario, D.; Lucarini, I.; Maita, F.; Ielmini, M.; Cataldi, M.E.; Cerroni, L.; Condò, R.; Maiolo, L. Towards Green Dentistry: Evaluating the Potential of 4D Printing for Sustainable Orthodontic Aligners with a Reduced Carbon Footprint. Polymers 2024, 16, 3566. [Google Scholar] [CrossRef] [Scilit]
- Robertson, L.; Kaur, H.; Fagundes, N.C.F.; Romanyk, D.; Major, P.; Flores Mir, C. Effectiveness of Clear Aligner Therapy for Orthodontic Treatment: A Systematic Review. Orthod. Craniofac. Res. 2020, 23, 133–142. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Ferlias, N.; Dalstra, M.; Cornelis, M.A.; Cattaneo, P.M. In Vitro Comparison of Different Invisalign® and 3Shape® Attachment Shapes to Control Premolar Rotation. Front. Bioeng. Biotechnol. 2022, 10, 840622. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Ahmed, M.M.A.; AbdelAllah, M.A.; Raslan, E.K.H.; Gouda, W.R.A.; Dawaba, M.M.M.; Abd El-Ghafar, I.; Ali, A.M.A.; Abdelmonem, M.H. Evaluation of Clear Aligners Attachment Success Rate with Different Composite Types. Int. J. Health Sci. 2021, 5, 533–541. [Google Scholar] [CrossRef] [Scilit]
- Chen, H.; Wei, S.; Wang, R.; Zhu, M. Improving the Physical-Mechanical Property of Dental Composites by Grafting Methacrylate-Polyhedral Oligomeric Silsesquioxane onto a Filler Surface. ACS Biomater. Sci. Eng. 2021, 7, 1428–1437. [Google Scholar] [CrossRef] [Scilit]
- Chen, M.H. Update on Dental Nanocomposites. J. Dent. Res. 2010, 89, 549–560. [Google Scholar] [CrossRef] [Scilit]
- Gazzani, F.; Bellisario, D.; Quadrini, F.; Danesi, C.; Alberti, A.; Cozza, P.; Pavoni, C. Light-Curing Process for Clear Aligners’ Attachment Reproduction: Comparison between Two Nanocomposites Cured by the Auxiliary of a New Tool. BMC Oral Health 2022, 22, 376. [Google Scholar] [CrossRef] [Scilit]
- Ferracane, J.L. Resin Composite—State of the Art. Dent. Mater. 2011, 27, 29–38. [Google Scholar] [CrossRef] [Scilit]
- Heintze, S.D.; Ilie, N.; Hickel, R.; Reis, A.; Loguercio, A.; Rousson, V. Laboratory Mechanical Parameters of Composite Resins and Their Relation to Fractures and Wear in Clinical Trials-A Systematic Review. Dent. Mater. 2017, 33, e101–e114. [Google Scholar] [CrossRef] [Scilit]
- Chen, W.; Qian, L.; Qian, Y.; Zhang, Z.; Wen, X. Comparative Study of Three Composite Materials in Bonding Attachments for Clear Aligners. Orthod. Craniofac. Res. 2021, 24, 520–527. [Google Scholar] [CrossRef] [Scilit]
- Ilie, N.; Hickel, R. Investigations on Mechanical Behaviour of Dental Composites. Clin. Oral Investig. 2009, 13, 427–438. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Bouchema, T.S.e.; Saunier, J.; Mollier, L.; Mauriello, J.; Savard, B.; Yagoubi, N. Comparison of Three Dental Resins for 3D Printing of Orthodontic Appliances: Comparison of Leaching, Biocompatibility, and Thermo-Mechanical Properties after Post-Curing and Aging. Dent. Mater. 2026, 42, 381–402. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Brockmann, W.; Geiß, P.L.; Klingen, J.; Schröder, B. Adhesive Bonding: Materials, Applications and Technology; John Wiley and Sons: Hoboken, NJ, USA, 2009; pp. 1–414. [Google Scholar] [CrossRef] [Scilit]
- Neoh, S.P.; Khantachawana, A.; Chintavalakorn, R.; Santiwong, P.; Srikhirin, T. Comparison of Physical, Mechanical, and Optical Properties between Thermoplastic Materials and 3-Dimensional Printing Resins for Orthodontic Clear Retainers. Am. J. Orthod. Dentofac. Orthop. 2025, 167, 95–109.e1. [Google Scholar] [CrossRef] [Scilit]
- Choi, J.Y.; Kim, H.; Kim, S.H.; Kim, S.J.; Cha, J.Y.; Lee, S.Y.; Lee, J.; Min, J.; Jang, S.; Khan, T.A.; et al. Mechanical and Viscoelastic Properties of a Temperature-Responsive Photocurable Resin for 3D Printed Orthodontic Clear Aligners. Sci. Rep. 2025, 15, 23530. [Google Scholar] [CrossRef] [Scilit]
- Daniele, V.; Macera, L.; Taglieri, G.; Di Giambattista, A.; Spagnoli, G.; Massaria, A.; Messori, M.; Quagliarini, E.; Chiappini, G.; Campanella, V.; et al. Thermoplastic Disks Used for Commercial Orthodontic Aligners: Complete Physicochemical and Mechanical Characterization. Materials 2020, 13, 2386. [Google Scholar] [CrossRef] [Scilit]
- Favero, R.; Zanetti, T.; Tosco, V.; Monterubbianesi, R.; Volpato, A. Mechanical Behaviour of Orthodontic Auxiliary Photopolymerisable Resins in Simulated Oral Conditions: An In Vitro Study. Dent. J. 2025, 13, 67. [Google Scholar] [CrossRef] [Scilit]
- Erbas, S.; Atik, E. A Comparative in Vitro Study of Different Composite Materials in Terms of Aligner Attachment Accuracy and Surface Roughness Using Different Curing Irradiances. Int. Orthod. 2025, 23, 100961. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Condò, R.; Mampieri, G.; Cioffi, A.; Pirelli, P.; Giancotti, A.; Maiolo, L.; Maita, F.; Convertino, A.; Lucarini, I.; Notargiacomo, A.; et al. Relationship between Reflectivity, Chemical Composition and Mechanical Behaviour of Orthodontic Bonding Nanofiller Resin Materials: A Proposal of an Alternative Method of Investigation. Appl. Sci. 2022, 12, 12538. [Google Scholar] [CrossRef] [Scilit]
- Alshali, R.Z.; Salim, N.A.; Satterthwaite, J.D.; Silikas, N. Post-Irradiation Hardness Development, Chemical Softening, and Thermal Stability of Bulk-Fill and Conventional Resin-Composites. J. Dent. 2015, 43, 209–218. [Google Scholar] [CrossRef] [Scilit]
- Good, P.; Cooper, T.; Querci, M.; Wiik, N.; Ambrosetti, G.; Steinfeld, A. Spectral Reflectance, Transmittance, and Angular Scattering of Materials for Solar Concentrators. Sol. Energy Mater. Sol. Cells 2016, 144, 509–522. [Google Scholar] [CrossRef] [Scilit]
- Parretta, A.; Yakubu, H.; Ferrazza, F. Method for Measurement of the Hemispherical/Hemispherical Reflectance of Photovoltaic Devices. Opt. Commun. 2001, 194, 17–32. [Google Scholar] [CrossRef] [Scilit]
- ElBatal, F.H.; Selim, M.S.; Marzouk, S.Y.; Azooz, M.A. UV-Vis Absorption of the Transition Metal-Doped SiO2-B2O3-Na2O Glasses. Phys. B 2007, 398, 126–134. [Google Scholar] [CrossRef] [Scilit]
- Wu, Y.; Hu, W.; Han, S. First-Principles Calculation of the Elastic Constants, the Electronic Density of States and the Ductility Mechanism of the Intermetallic Compounds: YAg, YCu and YRh. Phys. B 2008, 403, 3792–3797. [Google Scholar] [CrossRef] [Scilit]
- Zhang, Z.Q.; Liu, L.X.; Ye, Y.S.; Zhu, Z.B.; Qiao, Q.Y.; Dong, D.G.; Qian, Q.B.; Chen, C.D.; Zhou, Z.Q.; Qiu, Q.J. Cooperative Quantum Cutting in Yb3+-Tb3+ Codoped Borosilicate Glasses. IEEE Photonics Technol. Lett. 2009, 21, 1169–1171. [Google Scholar] [CrossRef]
- Kuznetsov, S.V.; Nizamutdinov, A.S.; Mayakova, M.N.; Voronov, V.V.; Madirov, E.I.; Khadiev, A.R.; Spassky, D.A.; Kamenskikh, I.A.; Yapryntsev, A.D.; Ivanov, V.K.; et al. Synthesis and Down-Conversion Luminescence of Ba4Y3F17:Yb:Pr Solid Solutions for Photonics. Nanosystems 2025, 10, 190–198. [Google Scholar] [CrossRef] [Scilit]
- Zhang, X.; Zhang, Y.; Zhang, X.; Yin, W.; Wang, Y.; Wang, H.; Lu, M.; Li, Z.; Gu, Z.; Yu, W.W. Yb3+ and Yb3+/Er3+ Doping for near-Infrared Emission and Improved Stability of CsPbCl3 Nanocrystals. J. Mater. Chem. C 2018, 6, 10101–10105. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Barik, S.; K.V., C.; Rani, R.; Kumar, K. Upconversion Emission Studies and Optical Thermometry in Tm3+, Yb3+ Co-Doped Cs2NaYCl6 Nanocrystals. J. Mol. Struct. 2026, 1349, 143943. [Google Scholar] [CrossRef] [Scilit]
- Wang, S.; Zhang, J. Effect of Titanium Dioxide (TiO2) on Largely Improving Solar Reflectance and Cooling Property of High Density Polyethylene (HDPE) by Influencing Its Crystallization Behavior. J. Alloys Compd. 2014, 617, 163–169. [Google Scholar] [CrossRef] [Scilit]
- Chiriac, A.P.; Nita, L.E.; Nistor, M.T. Nano-Network with Dual Temperature and pH Responsiveness Based on Copolymers of 2-Hydroxyethyl Methacrylate with 3,9-Divinyl-2,4,8,10-Tetraoxaspiro [5.5]-Undecane. J. Nanopart. Res. 2011, 13, 6953–6962. [Google Scholar] [CrossRef] [Scilit]
- Barszczewska-Rybarek, I.M. A Guide through the Dental Dimethacrylate Polymer Network Structural Characterization and Interpretation of Physico-Mechanical Properties. Materials 2019, 12, 4057. [Google Scholar] [CrossRef] [Scilit]
- Chen, B.; Lu, Z.; Meng, H.; Chen, Y.; Yang, L.; Zhang, H.; Xie, H.; Chen, C. Effectiveness of Pre-Silanization in Improving Bond Performance of Universal Adhesives or Self-Adhesive Resin Cements to Silica-Based Ceramics: Chemical and in Vitro Evidences. Dent. Mater. 2019, 35, 543–553. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Raszewski, Z.; Brząkalski, D.; Derpeński, Ł.; Jałbrzykowski, M.; Przekop, R.E. Aspects and Principles of Material Connections in Restorative Dentistry—A Comprehensive Review. Materials 2022, 15, 7131. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Zhang, X.; Zhang, Q.; Meng, X.; Ye, Y.; Feng, D.; Xue, J.; Wang, H.; Huang, H.; Wang, M.; Wang, J. Rheological and Mechanical Properties of Resin-Based Materials Applied in Dental Restorations. Polymers 2021, 13, 2975. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Ilie, N.; Hickel, R. Resin Composite Restorative Materials. Aust. Dent. J. 2011, 56, 59–66. [Google Scholar] [CrossRef] [Scilit]
- Al-Ahdal, K.; Silikas, N.; Watts, D.C. Rheological Properties of Resin Composites According to Variations in Composition and Temperature. Dent. Mater. 2014, 30, 517–524. [Google Scholar] [CrossRef] [Scilit]
- Gazzani, F.; Bellisario, D.; Pavoni, C.; Santo, L.; Cozza, P.; Lione, R. Comparative In Vitro Analysis of Composite Resins Used in Clear Aligner Attachments. Appl. Sci. 2025, 15, 8698. [Google Scholar] [CrossRef] [Scilit]
- Weckmann, J.; Scharf, S.; Graf, I.; Schwarze, J.; Keilig, L.; Bourauel, C.; Braumann, B. Influence of Attachment Bonding Protocol on Precision of the Attachment in Aligner Treatments. J. Orofac. Orthop. 2020, 81, 30–40. [Google Scholar] [CrossRef] [Scilit]
- Dasy, H.; Dasy, A.; Asatrian, G.; Rózsa, N.; Lee, H.F.; Kwak, J.H. Effects of Variable Attachment Shapes and Aligner Material on Aligner Retention. Angle Orthod. 2015, 85, 934–940. [Google Scholar] [CrossRef] [Scilit]
- Nucera, R.; Dolci, C.; Bellocchio, A.M.; Costa, S.; Barbera, S.; Rustico, L.; Farronato, M.; Militi, A.; Portelli, M. Effects of Composite Attachments on Orthodontic Clear Aligners Therapy: A Systematic Review. Materials 2022, 15, 533. [Google Scholar] [CrossRef] [Scilit]
- D’Antò, V.; Muraglie, S.; Castellano, B.; Candida, E.; Sfondrini, M.F.; Scribante, A.; Grippaudo, C. Influence of Dental Composite Viscosity in Attachment Reproduction: An Experimental in Vitro Study. Materials 2019, 12, 4001. [Google Scholar] [CrossRef] [Scilit]
- Nie, J.; Yap, A.U.; Wang, X.Y. Influence of Shrinkage and Viscosity of Flowable Composite Liners on Cervical Microleakage of Class II Restorations: A Micro-CT Analysis. Oper. Dent. 2018, 43, 656–664. [Google Scholar] [CrossRef] [Scilit]
- Petrovic, L.M.; Zorica, D.M.; Stojanac, I.L.; Krstonosic, V.S.; Hadnadjev, M.S.; Janev, M.B.; Premovic, M.T.; Atanackovic, T.M. Viscoelastic Properties of Uncured Resin Composites: Dynamic Oscillatory Shear Test and Fractional Derivative Model. Dent. Mater. 2015, 31, 1003–1009. [Google Scholar] [CrossRef] [Scilit]
- Mandall, N.A.; Hickman, J.; Macfarlane, T.V.; Mattick, R.C.R.; Millett, D.T.; Worthington, H.V. Adhesives for Fixed Orthodontic Brackets. Cochrane Database Syst. Rev. 2018, 4, CD002282. [Google Scholar] [CrossRef] [Scilit]
- Al Shamsi, A.H.; Cunningham, J.L.; Lamey, P.J.; Lynch, E. Three-Dimensional Measurement of Residual Adhesive and Enamel Loss on Teeth after Debonding of Orthodontic Brackets: An in-Vitro Study. Am. J. Orthod. Dentofac. Orthop. 2007, 131, 301.e9–301.e15. [Google Scholar] [CrossRef] [Scilit]
- Mantovani, E.; Castroflorio, E.; Rossini, G.; Garino, F.; Cugliari, G.; Deregibus, A.; Castroflorio, T. Scanning Electron Microscopy Analysis of Aligner Fitting on Anchorage Attachments. J. Orofac. Orthop. 2019, 80, 79–87. [Google Scholar] [CrossRef] [Scilit]
- Ravera, S.; Castroflorio, T.; Garino, F.; Daher, S.; Cugliari, G.; Deregibus, A. Maxillary Molar Distalization with Aligners in Adult Patients: A Multicenter Retrospective Study. Prog. Orthod. 2016, 17, 12. [Google Scholar] [CrossRef] [Scilit]
- Yangın, A.; Camcı, H.; Soybelli, M. Clear Aligner Attachments: A Comprehensive Review. Turk. J. Orthod. 2025, 38, 177–189. [Google Scholar] [CrossRef] [Scilit]
- Gold, B.P.; Siva, S.; Duraisamy, S.; Idaayath, A.; Kannan, R. Properties of Orthodontic Clear Aligner Materials—A Review. J. Evol. Med. Dent. Sci. 2021, 10, 3288–3294. [Google Scholar] [CrossRef] [Scilit]
- Iliadi, A.; Zervou, S.K.; Koletsi, D.; Schätzle, M.; Hiskia, A.; Eliades, T.; Eliades, G. Surface Alterations and Compound Release from Aligner Attachments in Vitro. Eur. J. Orthod. 2024, 46, cjae026. [Google Scholar] [CrossRef] [Scilit] [PubMed]
- Yildiz, H.; Dedeoglu, M. Reliability of Different Composite Materials in Aligner Treatments: A Comprehensıve in Vitro Study. Prog. Orthod. 2025, 26, 46. [Google Scholar] [CrossRef] [Scilit] [PubMed]









| Sample Name | Matrix Composition | Filler Composition |
|---|---|---|
| Aligner FLOW LC VOCO GmbH, Anton-Flettner-Str. 1–3, 27472 Cuxhaven, Germany) | HEDMA/Bis GMA/TEGDMA/BisEMA | Barium aluminum borosilicate glass, silica, pigments |
| SIMPLY SHADE Kerr Corporation, 200 S. Kraemer Blvd., Brea, CA 92821, USA (Part of Envista Holdings Corporation) | BisEMA/BisGMA/TEGDMA | Barium aluminum borosilicate glass, silica, ytterbium fluoride, pigments |
| SOFT ENA Flow Micerium S.p.A., Via Guglielmo Marconi, 83, 16036 Avegno (GE), Italy | UDMA/HEDMA | Silica, pigments |
| TETRIC EvoFlow Ivoclar Vivadent AG, S.r.l., Via Isonzo 69, 40033 Casalecchio di Reno (BO), Italy | DMA | Barium aluminum borosilicate glass, silica, ytterbium fluoride, titanium dioxide, pigments |
| VENUS Bulk Flow One Kulzer GmbH, Leipziger Str. 2, 63450 Hanau, Germany | EGBADMA/UDMA | Barium aluminum borosilicate glass, silica, ytterbium fluoride, titanium dioxide, pigments |
| Sample | Irradiation Time (s) t | Light Intensity (mW/cm2) I | Total Energy Density (J/cm2) E = t × I |
|---|---|---|---|
| VENUS | 20 | 1000 | 20 |
| SIMPLY SHADE | 20 | 1000 | 20 |
| SOFT ENA | 20 | 1000 | 20 |
| TETRIC | 10 | 1000 | 10 |
| Aligner FLOW | 20 | 1000 | 20 |
| Sample | Max Load at 0.25 mm (N) | Contact Stiffness (N/mm) | Elastic Modulus (MPa) |
|---|---|---|---|
| VENUS | 350 ± 10 | 1900 ± 80 | 550 ± 50 |
| TETRIC | 410 ± 20 | 2200 ± 100 | 610 ± 60 |
| SIMPLY SHADE | 590 ± 20 | 3500 ± 200 | 950 ± 80 |
| SOFT ENA | 12 ± 2 | 54 ± 6 | 19 ± 2 |
| Aligner FLOW | 270 ± 10 | 2400 ± 80 | 610 ± 70 |
Disclaimer/Publisher’s Note: The statements, opinions and data contained in all publications are solely those of the individual author(s) and contributor(s) and not of MDPI and/or the editor(s). MDPI and/or the editor(s) disclaim responsibility for any injury to people or property resulting from any ideas, methods, instructions or products referred to in the content. |
© 2026 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license.
Share and Cite
Palmieri, E.; Cataldi, M.E.; Cerroni, L.; Montaina, L.; Bonomo, M.; Petrone, G.; Bellisario, D.; Mattiello, L.; Pasquantonio, G.; Liscio, A.; et al. Rheological and Structural Evaluation of Dental Flowable Composites for Optimized Performance in Transparent Aligner Systems. Polymers 2026, 18, 1308. https://doi.org/10.3390/polym18111308
Palmieri E, Cataldi ME, Cerroni L, Montaina L, Bonomo M, Petrone G, Bellisario D, Mattiello L, Pasquantonio G, Liscio A, et al. Rheological and Structural Evaluation of Dental Flowable Composites for Optimized Performance in Transparent Aligner Systems. Polymers. 2026; 18(11):1308. https://doi.org/10.3390/polym18111308
Chicago/Turabian StylePalmieri, Elena, Maria Elena Cataldi, Loredana Cerroni, Luca Montaina, Matteo Bonomo, Gaetana Petrone, Denise Bellisario, Leonardo Mattiello, Guido Pasquantonio, Andrea Liscio, and et al. 2026. "Rheological and Structural Evaluation of Dental Flowable Composites for Optimized Performance in Transparent Aligner Systems" Polymers 18, no. 11: 1308. https://doi.org/10.3390/polym18111308
APA StylePalmieri, E., Cataldi, M. E., Cerroni, L., Montaina, L., Bonomo, M., Petrone, G., Bellisario, D., Mattiello, L., Pasquantonio, G., Liscio, A., Maita, F., Maiolo, L., & Condò, R. (2026). Rheological and Structural Evaluation of Dental Flowable Composites for Optimized Performance in Transparent Aligner Systems. Polymers, 18(11), 1308. https://doi.org/10.3390/polym18111308

