Applying SEM‐Based X‐ray Microtomography to Observe Self‐Healing in Solvent Encapsulated Thermoplastic Materials

In this work X-ray microtomography was used to observe fracture and healing processes in a liquid-based self-healing thermoplastic material. The method was able to produce data of sufficient resolution (<10µm) to observe~60mmmicrocapsules containing solvent within a polymeric material and in particular their behavior around a crack zone after fracture and healing. The reconstructed data showed the distribution of filled and several empty microcapsules within the matrix material. Additional color segmentation and 3D rendering of the data unambiguously demonstrated a large concentration of ruptured microcapsules near the fracture surfaces, covering-75mm span on both sides of the crack. A close investigation of the crack area confirmed the presence of healed and non-healed regions. Further analysis of the segmented data allowed a quantitative determination of the release of the encapsulated solvent.

[1]  N. Sottos,et al.  In situ poly(urea-formaldehyde) microencapsulation of dicyclopentadiene , 2003 .

[2]  Nancy R. Sottos,et al.  A Self‐Healing Poly(Dimethyl Siloxane) Elastomer , 2007 .

[3]  S. Wilkins,et al.  Quantitative X‐ray projection microscopy: phase‐contrast and multi‐spectral imaging , 2002, Journal of microscopy.

[4]  N. Sottos,et al.  In situ poly(urea-formaldehyde) microencapsulation of dicyclopentadiene , 2003, Journal of microencapsulation.

[5]  Nancy R. Sottos,et al.  Solvent-Promoted Self-Healing Epoxy Materials , 2007 .

[6]  Sanboh Lee,et al.  Ethanol‐induced crack healing in poly(methyl methacrylate) , 1994 .

[7]  J. Kruskal,et al.  COMPUTERIZED TOMOGRAPHY: THE NEW MEDICAL X-RAY TECHNOLOGY , 1978 .

[8]  E. Maire,et al.  On the application of x-ray microtomography in the field of materials science , 2001 .

[9]  Tao Yin,et al.  Self-healing woven glass fabric/epoxy composites with the healant consisting of micro-encapsulated epoxy and latent curing agent , 2008 .

[10]  S. Wilkins,et al.  Simultaneous phase and amplitude extraction from a single defocused image of a homogeneous object , 2002, Journal of microscopy.

[11]  N. Sottos,et al.  Autonomic healing of polymer composites , 2001, Nature.

[12]  S. Wilkins,et al.  X-ray phase-contrast microscopy and microtomography. , 2003, Optics express.

[13]  Ian Sinclair,et al.  In situ high resolution synchrotron x-ray tomography of fatigue crack closure micromechanisms , 2004 .

[14]  Sanboh Lee,et al.  Carbon tetrachloride‐induced crack healing in polycarbonate , 1994 .

[15]  E. Maire,et al.  Characterization of the morphology of cellular ceramics by 3D image processing of X-ray tomography , 2007 .

[16]  J. C. Elliott,et al.  X‐ray microtomography , 1982, Journal of microscopy.

[17]  Scott R White,et al.  A new self-healing epoxy with tungsten (VI) chloride catalyst , 2008, Journal of The Royal Society Interface.

[18]  Dhirendra Kumar,et al.  Preparation and characterization of microcapsules containing linseed oil and its use in self-healing coatings , 2008 .

[19]  Nancy R. Sottos,et al.  Effect of microcapsule size on the performance of self-healing polymers , 2007 .

[20]  C. Hansen Hansen Solubility Parameters: A User's Handbook , 1999 .

[21]  P. Cloetens,et al.  Holotomography: Quantitative phase tomography with micrometer resolution using hard synchrotron radiation x rays , 1999 .