journal article·2025-11-12Open access

Resonant Soft X-Ray Scattering Reveals Chromophore Domains in Polymer Doped with Disperse Orange 11 Dye

Elliot Steissberg, Acacia Patterson, Carson Beyers, Melanie Santiago, Mark G. Kuzyk, Brian A. Collins

Applied Sciences· Volume 15· Issue 22

Abstract

Chromophore domains were proposed in a previous work as the mediators of self-healing of optical properties in dye-doped polymers. A statistical mechanical model based on domains matches all observed self-healing dynamics as a function of dye concentration, temperature and light intensity. This suggests that domains are responsible. However, there is no direct observation of domains, nor has their physical morphology been determined. This work reports the first observation of domains in a self-healing polymer using resonant soft X-ray scattering (RSoXS), which gives a domain size in the range of 39.3 Å to 62.8 Å. This range includes the domain model’s prediction of an average domain size of roughly 30 molecules, which is about 56 Å, if the molecules form a loosely packed ball. X-ray scattering of samples of concentration spanning from neat polymer to the saturation limit of disperse orange 11 (DO11) dye in poly(methyl methacrylate) (PMMA) polymer shows domains in the expected size scales, with the mode of the effective scattering width varying little with concentration. However, for constant domain shape, the mode peak would decrease in q with increasing concentration, according to the domain model. This work suggests that the domain shape might change with concentration, which warrants further investigations of domain topology and geometry. The important evidence presented in this work is the direct experimental observation of domains, which is central to self-healing models.
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Research context

OpenAlex topics: Polymer composites and self-healing · Dyeing and Modifying Textile Fibers · Hydrogels: synthesis, properties, applications

SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.

Affiliations

Department of Physics and Astronomy, Washington State University, Pullman, WA 99164, USA

Department of Physics, University of Arizona, Tucson, AZ 85721, USA

Department of Astronomy and Astrophysics, University of California, San Diego, La Jolla, CA 92093, USA

References (87)

Show source-provided references
1. Second-order Nonlinear-optical Processes in Orientationally Ordered Materials: Relationship Between Molecular and Macroscopic Properties10.1364/JOSAB.4.000968 ↗
2. Lasing Action and Photodegradation of Disperse Orange 11 Dye in Liquid Solution10.1063/1.1791323 ↗
3. Molecular structure and reversible photodegradation in anthraquinone dyes10.1016/j.jphotochem.2016.05.011 ↗
4. Self-Healing Properties of 1-Amino,2,4-Dibromoanthraquinone Dye Doped in PMMA Polymer10.1021/acs.jpcc.6b10061 ↗
5. Duarte, F.J. (2024). Organic Lasers and Organic Photonics, IOP Publishing. [2nd ed.].10.1088/978-0-7503-5547-6 ↗
6. Laser-pumped Stimulated Emission from Organic Dyes: Experimental Studies and Analytical Comparisons10.1147/rd.112.0130 ↗
7. Time-Resolved Stimulated Emission Spectra of an Organic Dye Laser10.1063/1.1651925 ↗
8. Fletcher, A.N. (1981). FY 1980 Report on Dye Laser Materials.10.21236/ADA102882 ↗
9. An Investigation of the Thickness Variation of Spun-on Thin Films Commonly Associated with the Semiconductor Industry10.1149/1.2123749 ↗
10. Electro-optic polymer optical fibers and their device applications10.1117/12.454009 ↗
11. Demonstration of a self-healing all-polymer distributed Bragg reflector laser10.1063/1.5145148 ↗
12. Simple Synthesis of Elastomeric Photomechanical Switches That Self-Heal10.1002/marc.201800815 ↗
13. Shape-Memory and Self-Healing Effects in Mechanosalient Molecular Crystals10.1021/jacs.6b07406 ↗
14. Light-triggered self-healing and shape-memory polymers10.1039/c3cs35489j ↗
15. Polylactic acid promotes healing of photodegraded disperse orange 11 molecules10.1016/j.optmat.2017.12.007 ↗
16. Shape memory and self-healing materials from supramolecular block polymers10.1016/j.polymer.2017.11.043 ↗
17. Autonomic healing of polymer composites10.1038/35057232 ↗
18. The photochemistry of the self-healing chromophore Disperse Orange 1110.1002/poc.2907 ↗
19. Exarhos, G. (2011). Imaging studies of photodamage and self-healing of anthraquinone derivative dye doped polymers. SPIE Laser Damage Symposium Proceedings, SPIE. Number 16.
20. Photodegradation and self-healing in a Rhodamine 6G dye and Y2O3 nanoparticle-doped polyurethane random laser10.1007/s00340-015-6141-x ↗
21. Contributions of Multiphoton Absorption to Laser-Induced Intrinsic Damage in NaCl10.1063/1.88122 ↗
22. Phenomenological Theory of Laser Damage in Insulators10.1103/PhysRevB.20.3422 ↗
23. The Effect of Radiative Heat Lost on Laser Material Damage10.1063/1.340284 ↗
24. Investigation of Laser-Surface Interactions and Optical Damage Mechanisms Using Excitation by Pairs of Picosecond Laser Pulses10.1063/1.103660 ↗
25. One-dimensional Steady-state Model for Damage by Vaporization and Liquid Expulsion Due to Laser-material Interaction10.1063/1.339053 ↗
26. Chemical Precursor to Optical Damage Detected by Laser Ionization Mass Spectrometry10.1063/1.99766 ↗
27. Exarhos, G.J., Guenther, A.H., Kozlowski, M.R., and Soileau, M.J. (1998). Laser-Induced Damage in Optical Materials, SPIE.
28. A Closer Look at Laser Damage in PMMA10.1063/1.1655263 ↗
29. Recent Progress on Laser-Induced Modifications and Intrinsic Bulk Damage of Wide Gap Optical Materials10.1117/12.7977089 ↗
30. Ultrafast Imaging of Optical Damage Dynamics and Laser-Produced Wave Propagation in Polymethyl Methacrylate10.1063/1.341556 ↗
31. Laser-Induced Damage at 1064 nm, 125 psec10.1364/AO.16.001204 ↗
32. Mechanisms of Laser Damage to Transparent Polymer Materials
33. Single- and Multiple-shot Laser-damage Properties of Commercial Grade PMMA10.1364/AO.23.000682 ↗
34. Surface Laser Damage Thresholds Determined by photoacoustic Deflection10.1063/1.100491 ↗
35. Optical damage threshold of Au nanowires in strong femtosecond laser fields10.1364/OE.22.004235 ↗
36. Wood, R.M. (2003). Laser-Induced Damage of Optical Materials, Taylor & Francis.10.1887/0750308451 ↗
37. Wavelength dependence of 4-dimethylamino-4-nitrostilbene polymer thin film photodegradation10.1063/1.122035 ↗
38. Radiation Damage, Defects and Surfaces10.1016/0039-6028(79)90340-6 ↗
39. Mechanism of Damage of the Surface of a Transparent Dielectric during Illumination with Short Light Pulse10.1070/QE1973v002n04ABEH004452 ↗
40. The role of singlet oxygen in photodegradation of aminophenalenones10.1007/BF00660772 ↗
41. Amplified Spontaneous Emission and Recoverable Photodegradation in Disperse-Orange-11-Doped-Polymer10.1364/JOSAB.19.001790 ↗
42. Generalizing the correlated chromophore domain model of reversible photodegradation to include the effects of an applied electric field10.1103/PhysRevE.89.032601 ↗
43. A self healing model based on polymer-mediated chromophore correlations10.1063/1.4739295 ↗
44. Experimental tests of a new correlated chromophore domain model of self-healing in a dye-doped polymer10.1039/c3py00263b ↗
45. Imaging studies of photodamage and self-healing in disperse orange 11 dye-doped PMMA10.1364/JOSAB.28.000528 ↗
46. Imaging studies of temperature dependent photodegradation and self-healing in disperse orange 11 dye-doped polymers10.1063/1.4955201 ↗
47. A White Light Interferometric Microscope for Measuring Dose-Dependent Reversible Photodegradation10.1063/1.4822160 ↗
48. Zhang, M.Q., and Rong, M.Z. (2022). Extrinsic and Intrinsic Approaches to Self-Healing Polymers and Polymer Composites, Wiley.10.1002/9781119630005 ↗
49. Diffusion- and Mobility-Controlled Self-Healing Polymer Networks with Dynamic Covalent Bonding10.1021/acs.macromol.9b01453 ↗
50. Self-Healing of Unentangled Polymer Networks with Reversible Bonds10.1021/ma401111n ↗
51. Self-healing polymeric materials: A review of recent developments10.1016/j.progpolymsci.2008.02.001 ↗
52. Fluorescence Recovery after Two-Photon Bleaching for the Study of Dye Diffusion in Polymer Systems10.1021/ma034022s ↗
53. Testing the diffusion hypothesis as a mechanism of self-healing in Disperse Orange 11 doped in poly(methyl methacrylate)10.1364/JOSAB.28.002408 ↗
54. Mechanisms of reversible photodegradation in disperse orange 11 dye doped in PMMA polymer10.1063/1.2963502 ↗
55. Dichroism of Poly(Methyl Methacrylate) Thin Films Doped with Disperse Orange 11 Molecules10.12693/APhysPolA.115.857 ↗
56. Expanded Theory of H- and J-Molecular Aggregates: The Effects of Vibronic Coupling and Intermolecular Charge Transfer10.1021/acs.chemrev.7b00581 ↗
57. Reversible photodegradation of organic light-emitting diodes10.1063/1.1793344 ↗
58. Howell, B. (2001). Transient Absorption and Stimulated Emission of the Organic Dye Disperse Orange 11. [Ph.D. Thesis, Washington State University].
59. Self-healing organic-dye-based random lasers10.1364/OL.40.000577 ↗
60. Random lasing and reversible photodegradation in disperse orange 11 dye-doped PMMA with dispersed ZrO2 nanoparticles10.1088/2040-8978/18/1/015403 ↗
61. Recovery of photodegraded rhodamine 6g in ester-containing polymer matrices10.1039/c9pp00243j ↗
62. Roe, R.J. (2000). Methods of X-Ray and Neutron Scattering in Polymer Science, Oxford University Press.
63. In Situ and Operando X-ray Scattering Methods in Electrochemistry and Electrocatalysis10.1021/acs.chemrev.3c00331 ↗
64. Sub-Micrometer Structure Formation during Spin Coating Revealed by Time-Resolved In Situ Laser and X-Ray Scattering10.1002/adfm.201702516 ↗
65. Reconstructing the three-dimensional latent image of extreme ultraviolet resists with resonant soft X-ray scattering
66. Grazing-Incidence Soft-X-ray Scattering for the Chemical Structure Size Distribution Analysis in EUV Resist10.2494/photopolymer.35.61 ↗
67. X-Ray Interactions: Photoabsorption, Scattering, Transmission, and Reflection at E = 50–30,000 eV, Z = 1–9210.1006/adnd.1993.1013 ↗
68. Center for X-ray Optics and Advanced Light Source (2025, September 17). X-Ray Data Booklet, Available online: https://xdb.lbl.gov/.
69. Elemental fingerprinting of mineral species in iron-fortified milk: Anomalous small-angle X-ray scattering and resonant soft X-ray scattering studies10.1107/S1600577518007774 ↗
70. Resonant soft X-ray scattering in polymer science10.1002/pol.20210414 ↗
71. The utility of resonant soft x-ray scattering and reflectivity for the nanoscale characterization of polymers10.1140/epjst/e2009-00946-3 ↗
72. Water-Soluble Sacrificial Layers for Surface Micromachining10.1002/smll.200400159 ↗
73. X-Ray Scattering for Soft Matter Research at NSLS-II10.1080/08940886.2023.2207449 ↗
74. Nika: Software for two-dimensional data reduction10.1107/S0021889812004037 ↗
75. How to RSoXS10.1063/5.0267709 ↗
76. NEXAFS microscopy and resonant scattering: Composition and orientation probed in real and reciprocal space10.1016/j.polymer.2007.10.030 ↗
77. Ferri, F., Bertolotti, F., Guagliardi, A., and Masciocchi, N. (2020). Nanoparticle size distribution from inversion of wide angle X-ray total scattering data. Sci. Rep., 10.10.1038/s41598-020-69371-7 ↗
78. Anitas, E.M. (2020). Small-Angle Scattering from Fractals: Differentiating between Various Types of Structures. Symmetry, 12.10.3390/sym12010065 ↗
79. Hydrogen-Bonding-Mediated Molecular Vibrational Suppression for Enhancing the Fluorescence Quantum Yield Applicable for Visual Phenol Detection10.1021/acsami.1c15385 ↗
80. Dielectric Probe of Intermolecular Interactions in Poly(methyl methacrylate) (PMMA) and PMMA + SiO2 Matrixes Doped with Luminescent Organics10.1021/jp010618a ↗
81. Moldoveanu, S.C., and David, V. (2016). Selection of the HPLC Method in Chemical Analysis, Elsevier.
82. Spectroscopic studies of the mechanism of reversible photodegradation of 1-substituted aminoanthraquinone-doped polymers10.1063/1.4943963 ↗
83. Sampedro, D., and Sampedro Ruiz, D. (2019). Photoisomerization: Causes, Behavior and Effects, Nova Science Publishers. Chemistry research and applications.
84. Imaging conical intersection dynamics during azobenzene photoisomerization by ultrafast X-ray diffraction10.1073/pnas.2022037118 ↗
85. Multi-response optimization using Taguchi design and principle component analysis for removing binary mixture of alizarin red and alizarin yellow from aqueous solution by nano γ-alumina10.1016/j.saa.2014.01.100 ↗
86. Morphology Related Photodegradation of Low-Band-Gap Polymer Blends10.1002/aenm.201400497 ↗
87. CyRSoXS: A GPU-accelerated virtual instrument for polarized resonant soft X-ray scattering10.1107/S1600576723002790 ↗